DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:05:08 2018) ID: 2932; threads 39; handles 876; mem 518916.00 (1237824.00)kB; time: 1w 4d 22h 10m 38s MEMORY INFO: Memory PF:246.0, Ph:421.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.8,peak PF: 697.1, WS: 297.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:249.0, Ph:421.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.5,peak PF: 697.1, WS: 299.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:05:08 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000163 0.000158 0.000168 ) -0.068858 -0.065594 -0.010716 ( 0.000153 0.000148 0.000158 ) 0.109112 -0.153091 0.115835 ( 0.000229 0.000221 0.000236 ) 5.91502 ( 0.00943 ) 5.91640 ( 0.00956 ) 5.92265 ( 0.00879 ) 60.05206 ( 0.16263 ) 89.98756 ( 0.12553 ) 60.01743 ( 0.16786 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:05:08 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000163 0.000158 0.000168 ) -0.068858 -0.065594 -0.010716 ( 0.000153 0.000148 0.000158 ) 0.109112 -0.153091 0.115835 ( 0.000229 0.000221 0.000236 ) M - matrix: 0.021542 -0.014332 0.007143 ( 0.000059 0.000046 0.000043 ) -0.014332 0.028679 -0.014299 ( 0.000046 0.000071 0.000048 ) 0.007143 -0.014299 0.021472 ( 0.000043 0.000048 0.000062 ) unit cell: 5.915(9) 5.916(10) 5.923(9) 60.05(16) 89.99(13) 60.02(17) V = 146.7(3) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb PROFFITPEAK info: 371 peaks in the peak location table UB fit with 145 obs out of 160 (total:160,skipped:0) (90.63%) UB - matrix: -0.070103 0.030679 0.088730 ( 0.000144 0.000360 0.000276 ) -0.067907 -0.066756 -0.010219 ( 0.000163 0.000406 0.000312 ) 0.108857 -0.152456 0.115775 ( 0.000257 0.000641 0.000492 ) M - matrix: 0.021376 -0.014213 0.007077 ( 0.000064 0.000089 0.000069 ) -0.014213 0.028640 -0.014246 ( 0.000089 0.000204 0.000113 ) 0.007077 -0.014246 0.021381 ( 0.000069 0.000113 0.000124 ) unit cell: 5.927(19) 5.91(2) 5.933(16) 60.1(3) 90.0(2) 60.2(3) V = 147.4(7) UB fit with 145 obs out of 160 (total:160,skipped:0) (90.63%) UB - matrix: -0.070103 0.030679 0.088730 ( 0.000144 0.000360 0.000276 ) -0.067907 -0.066756 -0.010219 ( 0.000163 0.000406 0.000312 ) 0.108857 -0.152456 0.115775 ( 0.000257 0.000641 0.000492 ) M - matrix: 0.021376 -0.014213 0.007077 ( 0.000064 0.000089 0.000069 ) -0.014213 0.028640 -0.014246 ( 0.000089 0.000204 0.000113 ) 0.007077 -0.014246 0.021381 ( 0.000069 0.000113 0.000124 ) unit cell: 5.927(19) 5.91(2) 5.933(16) 60.1(3) 90.0(2) 60.2(3) V = 147.4(7) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070192 0.030522 0.088679 ( 0.000162 0.000404 0.000309 ) -0.068040 -0.066710 -0.010154 ( 0.000155 0.000387 0.000296 ) 0.109086 -0.153126 0.116287 ( 0.000240 0.000598 0.000458 ) M - matrix: 0.021456 -0.014307 0.007152 ( 0.000061 0.000085 0.000066 ) -0.014307 0.028829 -0.014423 ( 0.000085 0.000192 0.000107 ) 0.007152 -0.014423 0.021490 ( 0.000066 0.000107 0.000120 ) UB fit with 146 obs out of 160 (total:160,skipped:0) (91.25%) unit cell: 5.920(18) 5.909(19) 5.937(16) 59.8(3) 90.0(2) 60.2(3) V = 146.8(7) UB fit with 146 obs out of 160 (total:160,skipped:0) (91.25%) UB - matrix: -0.070192 0.030522 0.088679 ( 0.000162 0.000404 0.000309 ) -0.068040 -0.066710 -0.010154 ( 0.000155 0.000387 0.000296 ) 0.109086 -0.153127 0.116287 ( 0.000240 0.000598 0.000458 ) M - matrix: 0.021456 -0.014307 0.007152 ( 0.000061 0.000085 0.000066 ) -0.014307 0.028830 -0.014423 ( 0.000085 0.000192 0.000107 ) 0.007152 -0.014423 0.021490 ( 0.000066 0.000107 0.000120 ) unit cell: 5.920(18) 5.909(19) 5.937(16) 59.8(3) 90.0(2) 60.2(3) V = 146.8(7) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070260 0.030630 0.088667 ( 0.000162 0.000402 0.000308 ) -0.068114 -0.066668 -0.010147 ( 0.000155 0.000385 0.000295 ) 0.109116 -0.153261 0.116377 ( 0.000241 0.000599 0.000459 ) M - matrix: 0.021482 -0.014334 0.007160 ( 0.000061 0.000085 0.000066 ) -0.014334 0.028872 -0.014444 ( 0.000085 0.000192 0.000108 ) 0.007160 -0.014444 0.021508 ( 0.000066 0.000108 0.000120 ) UB fit with 146 obs out of 160 (total:160,skipped:0) (91.25%) unit cell: 5.918(18) 5.907(19) 5.935(16) 59.8(3) 90.0(2) 60.1(3) V = 146.6(7) 160 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Run 1 Omega scan: (-107.000 - -82.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.841) HKL list info: 271 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070260 0.030630 0.088667 ( 0.000162 0.000402 0.000308 ) -0.068114 -0.066668 -0.010147 ( 0.000155 0.000385 0.000295 ) 0.109116 -0.153261 0.116377 ( 0.000241 0.000599 0.000459 ) M - matrix: 0.021482 -0.014334 0.007160 ( 0.000061 0.000085 0.000066 ) -0.014334 0.028872 -0.014444 ( 0.000085 0.000192 0.000108 ) 0.007160 -0.014444 0.021509 ( 0.000066 0.000108 0.000120 ) UB fit with 146 obs out of 160 (total:160,skipped:0) (91.25%) unit cell: 5.918(18) 5.907(19) 5.935(16) 59.8(3) 90.0(2) 60.1(3) V = 146.6(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 146 obs out of 160 (total:160,skipped:0) (91.25%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb 3 of 89 peaks identified as outliers and rejected 86 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 86 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 86 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.49- 1.28 | 9 | 1.012 ( 0.191) | 1.140 ( 0.458) | 1.537 ( 0.967) | 1.26- 1.09 | 9 | 1.054 ( 0.118) | 1.083 ( 0.110) | 0.921 ( 0.371) | 1.09- 0.92 | 9 | 1.067 ( 0.086) | 1.069 ( 0.117) | 1.147 ( 0.404) | 0.92- 0.86 | 9 | 1.108 ( 0.116) | 1.067 ( 0.107) | 1.166 ( 0.523) | 0.84- 0.78 | 9 | 1.149 ( 0.062) | 1.038 ( 0.116) | 1.496 ( 0.512) | 0.78- 0.73 | 9 | 1.117 ( 0.097) | 0.977 ( 0.147) | 1.730 ( 0.482) | 0.73- 0.69 | 9 | 1.125 ( 0.046) | 0.932 ( 0.120) | 1.464 ( 0.421) | 0.69- 0.66 | 9 | 1.112 ( 0.042) | 0.891 ( 0.123) | 1.404 ( 0.504) | 0.65- 0.61 | 9 | 1.113 ( 0.032) | 0.834 ( 0.025) | 1.797 ( 0.663) | 0.61- 0.59 | 5 | 1.045 ( 0.060) | 0.783 ( 0.025) | 1.080 ( 0.417) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.49- 0.59 | 86 | 1.092 ( 0.106) | 0.991 ( 0.210) | 1.388 ( 0.620) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 86 obs out of 86 (total:86,skipped:0) (100.00%) UB - matrix: -0.069991 0.030009 0.089138 ( 0.000067 0.000156 0.000116 ) -0.068654 -0.065570 -0.010827 ( 0.000079 0.000184 0.000137 ) 0.109331 -0.153718 0.116449 ( 0.000080 0.000188 0.000140 ) M - matrix: 0.021565 -0.014405 0.007236 ( 0.000023 0.000030 0.000023 ) -0.014405 0.028829 -0.014515 ( 0.000030 0.000063 0.000035 ) 0.007236 -0.014515 0.021623 ( 0.000023 0.000035 0.000039 ) unit cell: 5.917(8) 5.927(8) 5.928(6) 59.72(13) 89.93(10) 60.03(14) V = 146.6(3) OTKP changes: 86 1 1 1 UB - matrix: -0.070168 0.030667 0.088975 ( 0.000048 0.000111 0.000083 ) -0.068486 -0.066098 -0.010558 ( 0.000072 0.000169 0.000126 ) 0.109341 -0.153891 0.116689 ( 0.000077 0.000181 0.000134 ) M - matrix: 0.021569 -0.014452 0.007239 ( 0.000021 0.000027 0.000021 ) -0.014452 0.028992 -0.014531 ( 0.000027 0.000060 0.000032 ) 0.007239 -0.014531 0.021644 ( 0.000021 0.000032 0.000035 ) UB fit with 86 obs out of 86 (total:86,skipped:0) (100.00%) unit cell: 5.918(7) 5.904(7) 5.919(5) 59.83(11) 89.98(8) 60.01(13) V = 145.9(2) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -82.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.826) HKL list info: 269 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 86 obs out of 86 (total:86,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb 3 of 93 peaks identified as outliers and rejected 90 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 90 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 90 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.50- 1.27 | 9 | 1.014 ( 0.193) | 1.167 ( 0.526) | 1.547 ( 0.978) | 1.26- 1.09 | 9 | 1.041 ( 0.110) | 1.072 ( 0.106) | 0.895 ( 0.377) | 1.09- 0.92 | 9 | 1.080 ( 0.092) | 1.092 ( 0.137) | 1.137 ( 0.406) | 0.92- 0.87 | 9 | 1.077 ( 0.112) | 1.059 ( 0.109) | 0.964 ( 0.316) | 0.85- 0.81 | 9 | 1.164 ( 0.057) | 1.059 ( 0.099) | 1.655 ( 0.476) | 0.81- 0.75 | 9 | 1.111 ( 0.101) | 0.977 ( 0.145) | 1.523 ( 0.500) | 0.73- 0.71 | 9 | 1.121 ( 0.043) | 0.938 ( 0.118) | 1.581 ( 0.509) | 0.70- 0.67 | 9 | 1.126 ( 0.044) | 0.897 ( 0.085) | 1.427 ( 0.446) | 0.67- 0.63 | 9 | 1.114 ( 0.032) | 0.834 ( 0.032) | 1.916 ( 0.451) | 0.62- 0.59 | 9 | 1.076 ( 0.064) | 0.813 ( 0.039) | 1.138 ( 0.511) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.50- 0.59 | 90 | 1.093 ( 0.105) | 0.991 ( 0.223) | 1.378 ( 0.612) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-14.2 | 9 | 1.118 ( 0.042) | 1.130 ( 0.075) | 1.353 ( 0.594) | 15.2-18.2 | 9 | 1.163 ( 0.088) | 1.310 ( 0.452) | 1.374 ( 0.903) | 19.5-21.9 | 9 | 1.151 ( 0.076) | 1.072 ( 0.068) | 1.494 ( 0.536) | 22.5-28.5 | 9 | 1.127 ( 0.057) | 1.088 ( 0.118) | 1.395 ( 0.536) | 28.7-30.2 | 9 | 1.114 ( 0.073) | 0.983 ( 0.135) | 1.501 ( 0.574) | 30.9-34.1 | 9 | 1.085 ( 0.085) | 0.895 ( 0.065) | 1.333 ( 0.546) | 34.6-36.8 | 9 | 1.077 ( 0.097) | 0.889 ( 0.083) | 1.645 ( 0.617) | 37.0-39.4 | 9 | 1.069 ( 0.062) | 0.916 ( 0.079) | 1.266 ( 0.477) | 39.5-42.4 | 9 | 0.993 ( 0.147) | 0.813 ( 0.058) | 1.191 ( 0.537) | 42.6-49.4 | 9 | 1.029 ( 0.136) | 0.809 ( 0.053) | 1.233 ( 0.552) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.4 | 90 | 1.093 ( 0.105) | 0.991 ( 0.223) | 1.378 ( 0.612) | Fitted profile normalization line parameters e1 dimension: a=-0.0006 b=1.05 e2 dimension: a=-0.0101 b=1.26 e3 dimension: a=0.0095 b=0.89 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7487 lp-corr: 4099 Maximum peak integral for reflections I/sig<= 100 - raw: 485618 lp-corr: 697824 Maximum peak integral for reflections I/sig<= 10000 - raw: 4965442 lp-corr: 2108394 PROFFITPEAK - Finished at Tue Mar 27 13:05:10 2018 PROFFITMAIN - Started at Tue Mar 27 13:05:10 2018 OTKP changes: 90 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 90 1 1 1 UB - matrix: -0.070174 0.030697 0.088952 ( 0.000045 0.000108 0.000080 ) -0.068486 -0.066057 -0.010590 ( 0.000068 0.000163 0.000122 ) 0.109332 -0.153857 0.116660 ( 0.000073 0.000175 0.000131 ) M - matrix: 0.021568 -0.014452 0.007238 ( 0.000019 0.000026 0.000020 ) -0.014452 0.028978 -0.014519 ( 0.000026 0.000059 0.000031 ) 0.007238 -0.014519 0.021634 ( 0.000020 0.000031 0.000034 ) UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) unit cell: 5.919(7) 5.905(7) 5.919(5) 59.85(10) 89.99(8) 60.00(12) V = 146.0(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -82.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.828) HKL list info: 281 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070174 0.030697 0.088952 ( 0.000045 0.000108 0.000080 ) -0.068486 -0.066057 -0.010590 ( 0.000068 0.000163 0.000122 ) 0.109332 -0.153857 0.116660 ( 0.000073 0.000175 0.000131 ) M - matrix: 0.021568 -0.014452 0.007238 ( 0.000019 0.000026 0.000020 ) -0.014452 0.028978 -0.014519 ( 0.000026 0.000059 0.000031 ) 0.007238 -0.014519 0.021634 ( 0.000020 0.000031 0.000034 ) UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) unit cell: 5.919(7) 5.905(7) 5.919(5) 59.85(10) 89.99(8) 60.00(12) V = 146.0(2) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070174 0.030697 0.088952 ( 0.000045 0.000108 0.000080 ) -0.068486 -0.066057 -0.010590 ( 0.000068 0.000163 0.000122 ) 0.109332 -0.153857 0.116660 ( 0.000073 0.000175 0.000131 ) M - matrix: 0.021568 -0.014452 0.007238 ( 0.000019 0.000026 0.000020 ) -0.014452 0.028978 -0.014519 ( 0.000026 0.000059 0.000031 ) 0.007238 -0.014519 0.021634 ( 0.000020 0.000031 0.000034 ) UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) unit cell: 5.919(7) 5.905(7) 5.919(5) 59.85(10) 89.99(8) 60.00(12) V = 146.0(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 7 reflections under beam stop or inside a detector rejection region 1 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof 125 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:05:11 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 1bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -82.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.828) PROFFIT INFO: signal sum: min=121.0000 max=10870367.0000 PROFFIT INFO: signal sum lp corr: min=814.3329 max=1751893.6379 PROFFIT INFO: background sum: min=1683.0000 max=8205.0000 PROFFIT INFO: background sum sig2: min=652.0000 max=6209.0000 PROFFIT INFO: num of signal pixels: min=63 max=519 PROFFIT INFO: Inet: min=1302.9326 max=2803029.7500 PROFFIT INFO: sig(Inet): min=353.2547 max=45085.2188 PROFFIT INFO: Inet/sig(Inet): min=1.07 max=221.15 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 1 3 15 31 32 50 82 113 125 Percent 0.0 0.0 0.8 2.4 12.0 24.8 25.6 40.0 65.6 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 125 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 125 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2803030- 1339143 12 1895201.25 126.35 100.00 1329527- 821358 12 1013297.67 112.06 100.00 816223- 272625 12 496322.92 93.04 100.00 264112- 186246 12 218500.23 74.72 100.00 176160- 154798 12 161805.18 53.14 100.00 150812- 102729 12 125579.15 37.48 100.00 102312- 81150 12 90546.22 31.18 100.00 78605- 6431 12 50554.89 23.71 100.00 6330- 3637 12 5006.69 4.93 91.67 3603- 1303 17 2764.30 3.84 88.24 ------------------------------------------------------------------------------------ 2803030- 1303 125 389830.11 53.96 97.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 628563.93 79.80 100.00 1.32- 1.12 12 783064.42 70.23 100.00 1.09- 0.93 12 524331.57 85.28 100.00 0.92- 0.88 12 346297.40 62.49 100.00 0.85- 0.80 12 597657.79 75.74 100.00 0.80- 0.75 12 230469.78 38.25 100.00 0.73- 0.71 12 150546.02 32.29 100.00 0.71- 0.67 12 332025.82 46.12 91.67 0.67- 0.64 12 251190.16 35.76 100.00 0.64- 0.60 17 152882.42 25.48 88.24 ------------------------------------------------------------------------------------ 4.82- 0.60 125 389830.11 53.96 97.60 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:05:11 2018 Sorting 125 observations 0 unique observations with > 7.00 F2/sig(F2) 125 observations in 1 runs Run # start # end # total # 1 1 23 23 Total number of frames 23 Maximum number of 0 frame scales suggested for reliable scaling Can't fit requested scale/empirical absorption model (pTmpToScale3AbspackHKL) ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 0, Friedel: 1 Min/max for: run:1/1 frame:2/24 125 reflections read from tmp file 125 reflections are rejected (0 as outliers, 125 as groups of 1 refl) ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2803030- 1339143 12 1895201.25 126.35 100.00 1329527- 821358 12 1013297.67 112.06 100.00 816223- 272625 12 496322.92 93.04 100.00 264112- 186246 12 218500.23 74.72 100.00 176160- 154798 12 161805.18 53.14 100.00 150812- 102729 12 125579.15 37.48 100.00 102312- 81150 12 90546.22 31.18 100.00 78605- 6431 12 50554.89 23.71 100.00 6330- 3637 12 5006.69 4.93 91.67 3603- 1303 17 2764.30 3.84 88.24 ------------------------------------------------------------------------------------ 2803030- 1303 125 389830.11 53.96 97.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 628563.93 79.80 100.00 1.32- 1.12 12 783064.42 70.23 100.00 1.09- 0.93 12 524331.57 85.28 100.00 0.92- 0.88 12 346297.40 62.49 100.00 0.85- 0.80 12 597657.79 75.74 100.00 0.80- 0.75 12 230469.78 38.25 100.00 0.73- 0.71 12 150546.02 32.29 100.00 0.71- 0.67 12 332025.82 46.12 91.67 0.67- 0.64 12 251190.16 35.76 100.00 0.64- 0.60 17 152882.42 25.48 88.24 ------------------------------------------------------------------------------------ 4.82- 0.60 125 389830.11 53.96 97.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 628563.93 79.80 100.00 4.82- 1.12 24 705814.17 75.01 100.00 4.82- 0.93 36 645319.97 78.44 100.00 4.82- 0.88 48 570564.33 74.45 100.00 4.82- 0.80 60 575983.02 74.71 100.00 4.82- 0.75 72 518397.48 68.63 100.00 4.82- 0.71 84 465847.27 63.44 100.00 4.82- 0.67 96 449119.59 61.27 98.96 4.82- 0.64 108 427127.43 58.44 99.07 4.82- 0.60 125 389830.11 53.96 97.60 ------------------------------------------------------------------------------------ 4.82- 0.60 125 389830.11 53.96 97.60 Scale applied to data: s=0.356756 (maximum obs:2803029.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.000; Rsigma 0.013: data 125 -> merged 125 With outlier rejection... Rint 0.000; Rsigma 0.013: data 125 -> merged 125 Rejected total: 0, method kkm 0, method Blessing 0 Completeness direct cell (a, b, c) = (5.919, 5.905, 5.919), (alpha, beta, gamma) = (59.848, 89.988, 60.003) wavelength: 0.709300 dmin, dmax value (Ang): 0.597866, 4.829729 completeness table (Laue group: P1, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.32 13 137 1.00 9.49 13 1.32 - 1.02 17 137 1.00 12.41 17 1.02 - 0.91 11 137 1.00 8.03 11 0.91 - 0.82 15 137 1.00 10.95 15 0.82 - 0.76 12 137 1.00 8.76 12 0.76 - 0.72 12 137 1.00 8.76 12 0.72 - 0.68 10 137 1.00 7.30 10 0.68 - 0.65 13 137 1.00 9.49 13 0.65 - 0.63 9 137 1.00 6.57 9 0.63 - 0.60 7 137 1.00 5.11 7 --------------------------------------------------------------- 5.92 - 0.60 119 1370 1.00 8.69 119 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:05:11 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918870 5.905407 5.919111 59.8479 89.9883 60.0030 125 Reflections read from file xs1714a.hkl; mean (I/sigma) = 53.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 59 61 64 62 92 85 90 125 N (int>3sigma) = 0 58 61 63 62 91 84 89 122 Mean intensity = 0.0 13.7 5.7 13.1 13.2 10.9 16.4 14.2 13.9 Mean int/sigma = 0.0 50.3 50.1 50.5 51.7 50.3 61.2 57.2 54.0 Lattice type: P chosen Volume: 145.98 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.899 5.905 5.907 90.26 119.82 119.81 Niggli form: a.a = 34.794 b.b = 34.874 c.c = 34.892 b.c = -0.159 a.c = -17.326 a.b = -17.316 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.344 CUBIC F-lattice R(int) = 0.020 [ 31] Vol = 583.9 Cell: 8.372 8.370 8.334 90.13 89.99 90.00 Volume: 583.92 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.312 RHOMBOHEDRAL R-lattice R(int) = 0.218 [ 9] Vol = 437.9 Cell: 5.919 5.905 14.489 90.16 90.04 120.15 Volume: 437.94 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.312 RHOMBOHEDRAL R-lattice R(int) = 0.000 [ 0] Vol = 437.9 Trigonal Cell: 5.919 5.905 14.489 90.16 90.04 120.15 Volume: 437.94 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.126 TETRAGONAL I-lattice R(int) = 0.021 [ 4] Vol = 292.0 Cell: 5.919 5.919 8.334 89.92 89.90 90.01 Volume: 291.96 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.106 TETRAGONAL I-lattice R(int) = 0.021 [ 4] Vol = 292.0 Cell: 5.919 5.919 8.334 90.10 90.08 90.01 Volume: 291.96 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 25] Vol = 292.0 Cell: 5.919 5.919 8.334 89.90 89.92 90.01 Volume: 291.96 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.109 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 4] Vol = 292.0 Cell: 5.899 8.372 5.912 89.99 89.75 90.01 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.080 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 5.919 5.919 8.334 90.08 90.10 90.01 Volume: 291.96 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.203 MONOCLINIC I-lattice R(int) = 0.036 [ 3] Vol = 292.0 Cell: 5.899 5.912 8.372 90.01 90.01 90.25 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.019 MONOCLINIC I-lattice R(int) = 0.031 [ 4] Vol = 292.0 Cell: 5.899 8.372 5.912 89.99 90.25 89.99 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.108 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 5.912 5.899 8.372 89.99 90.01 89.75 Volume: 291.96 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.275 MONOCLINIC C-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 10.237 5.905 5.907 90.26 125.15 89.77 Volume: 291.96 Matrix: 0.0000 -1.0000 2.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.0 Cell: 5.899 5.905 5.907 90.26 119.82 119.81 Volume: 145.98 Matrix: 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 61 0 85 82 125 N (int>3sigma) = 0 0 0 0 61 0 84 80 122 Mean intensity = 0.0 0.0 0.0 0.0 5.7 0.0 16.4 13.4 13.9 Mean int/sigma = 0.0 0.0 0.0 0.0 50.1 0.0 61.2 49.5 54.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.245 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 2 2 6 28 N I>3s 2 2 5 28 0.1 0.1 0.1 6.7 6.3 6.3 6.8 58.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.020 31 Fd-3m 1 1 227 C N N N N 37 2284 0.028 47 0kl, h0l, hk0, with too little data to consider diffraction symbol Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371571 8.369862 8.333516 90.1334 89.9855 89.9977 ZERR 1.00 0.002515 0.013964 0.033465 0.0284 0.1067 0.0215 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: P-1 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2803030- 816223 25 25 25 1.0 1428728.41 117.84 0.000 0.000 792681- 172717 25 25 25 1.0 324421.23 83.00 0.000 0.000 168947- 98565 25 25 25 1.0 136092.21 41.37 0.000 0.000 92662- 5735 25 25 25 1.0 56580.44 23.40 0.000 0.000 5496- 1303 25 25 25 1.0 3328.25 4.17 0.000 0.000 ------------------------------------------------------------------------------------------- 2803030- 1303 125 125 125 1.0 389830.11 53.96 0.000 0.000 Statistics vs resolution - point group symmetry: P-1 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.09 25 25 25 1.0 685031.44 74.98 0.000 0.000 0.013 1.09-0.85 25 25 25 1.0 523753.94 79.10 0.000 0.000 0.009 0.84-0.73 25 25 25 1.0 295108.51 47.69 0.000 0.000 0.013 0.73-0.65 25 25 25 1.0 263684.26 40.13 0.000 0.000 0.016 0.65-0.60 25 25 25 1.0 181572.40 27.88 0.000 0.000 0.020 ------------------------------------------------------------------------------------------------------ inf-0.60 125 125 125 1.0 389830.11 53.96 0.000 0.000 0.013 inf-0.61 119 119 119 1.0 407314.90 55.95 0.000 0.000 0.013 Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.09 25 234 25 10.7 1.0 685031.44 74.98 0.000 0.000 1.09-0.85 25 237 25 10.5 1.0 523753.94 79.10 0.000 0.000 0.84-0.73 25 258 25 9.7 1.0 295108.51 47.69 0.000 0.000 0.73-0.65 25 316 25 7.9 1.0 263684.26 40.13 0.000 0.000 0.65-0.60 25 344 25 7.3 1.0 181572.40 27.88 0.000 0.000 -------------------------------------------------------------------------------------------- inf-0.60 125 1413 125 8.8 1.0 389830.11 53.96 0.000 0.000 inf-0.61 119 1348 119 8.8 1.0 407314.90 55.95 0.000 0.000 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 -1.0 0.0 1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 -1.0 0.0 1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.024738 0.079563 -0.015349 ( 0.000016 0.000027 0.000054 ) -0.072566 0.028948 0.033028 ( 0.000024 0.000041 0.000082 ) 0.036068 0.003664 0.076929 ( 0.000026 0.000044 0.000088 ) M - matrix: 0.007179 -0.000000 -0.000002 ( 0.000004 0.000004 0.000007 ) -0.000000 0.007182 0.000017 ( 0.000004 0.000005 0.000006 ) -0.000002 0.000017 0.007244 ( 0.000007 0.000006 0.000015 ) Constraint UB - matrix: 0.024738 0.079563 -0.015349 ( 0.000016 0.000027 0.000054 ) -0.072566 0.028948 0.033028 ( 0.000024 0.000041 0.000082 ) 0.036068 0.003664 0.076929 ( 0.000026 0.000044 0.000088 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) unit cell: 8.372(5) 8.370(3) 8.334(7) 90.13(4) 89.99(6) 90.00(4) V = 583.9(6) unit cell: 8.3583(6) 8.3583(6) 8.3583(6) 90.0 90.0 90.0 V = 583.92(7) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -82.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.828) PROFFIT INFO: signal sum: min=121.0000 max=10870367.0000 PROFFIT INFO: signal sum lp corr: min=814.3329 max=1751893.6379 PROFFIT INFO: background sum: min=1683.0000 max=8205.0000 PROFFIT INFO: background sum sig2: min=652.0000 max=6209.0000 PROFFIT INFO: num of signal pixels: min=63 max=519 PROFFIT INFO: Inet: min=1302.9326 max=2803029.7500 PROFFIT INFO: sig(Inet): min=353.2547 max=45085.2188 PROFFIT INFO: Inet/sig(Inet): min=1.07 max=221.15 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 2 6 30 62 64 100 164 226 250 Percent 0.0 0.0 0.8 2.4 12.0 24.8 25.6 40.0 65.6 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 125 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 125 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2803030- 1339143 12 1895201.25 126.35 100.00 1329527- 821358 12 1013297.67 112.06 100.00 816223- 272625 12 496322.92 93.04 100.00 264112- 186246 12 218500.23 74.72 100.00 176160- 154798 12 161805.18 53.14 100.00 150812- 102729 12 125579.15 37.48 100.00 102312- 81150 12 90546.22 31.18 100.00 78605- 6431 12 50554.89 23.71 100.00 6330- 3637 12 5006.69 4.93 91.67 3603- 1303 17 2764.30 3.84 88.24 ------------------------------------------------------------------------------------ 2803030- 1303 125 389830.11 53.96 97.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 628563.93 79.80 100.00 1.32- 1.11 12 783064.42 70.23 100.00 1.09- 0.93 12 524331.57 85.28 100.00 0.92- 0.87 12 346297.40 62.49 100.00 0.85- 0.80 12 597657.79 75.74 100.00 0.80- 0.75 12 230469.78 38.25 100.00 0.73- 0.71 12 150546.02 32.29 100.00 0.71- 0.67 12 334797.46 46.43 91.67 0.67- 0.64 12 248418.51 35.45 100.00 0.64- 0.60 17 152882.42 25.48 88.24 ------------------------------------------------------------------------------------ 4.82- 0.60 125 389830.11 53.96 97.60 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:05:12 2018 Sorting 125 observations 29 unique observations with > 7.00 F2/sig(F2) 125 observations in 1 runs Run # start # end # total # 1 1 23 23 Total number of frames 23 Maximum number of 29 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 125 observations in 1 runs Run # start # end # total # 1 1 23 23 Total number of frames 23 95 observations > 7.00 F2/sig(F2) 95 observations in 1 runs Run # start # end # total # 1 1 23 23 Total number of frames 23 Removing 'redundancy=1' reflections Average redundancy: 2.2 (Out of 95 removed 31 = 64, unique = 29) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 64 observations in 1 runs Run # start # end # total # 1 1 23 23 Total number of frames 23 Frame #3 of 23 skipped from refinement Frame #14 of 23 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 29 unique data precomputed (should be 29) 29 unique data with 64 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.2 (Out of 64 removed 0 = 64, unique = 29) 29 unique data precomputed (should be 29) 29 unique data with 64 observations RMS deviation of equivalent data = 0.03534 Rint = 0.02794 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.02794, wR= 0.04348 Trying model 1 (ne=2, no=0)... Results: Rint= 0.01735, wR= 0.02346, Acormin=0.935, Acormax=1.117, Acor_av=0.995 F test: Probability=0.986, F= 2.222 Trying model 2 (ne=2, no=1)... Results: Rint= 0.01715, wR= 0.02265, Acormin=0.925, Acormax=1.096, Acor_av=0.996 F test: Probability=0.000, F= 0.921 Final absorption model (ne=2, no=0): Rint= 0.01735, Acormin=0.935, Acormax=1.117, Acor_av=0.995 Combined refinement in use Rint: 0.02815 There are 21 active scales (one needs to be fixed) Refinement control: frame scale #2 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 25 pars with 325 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.03534 Using Levenberg-Marquardt: 0.00010 New wR= 0.01195 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.02794 with corrections 0.01087 Rint for all data: 0.02815 with corrections 0.01115 0 observations identified as outliers and rejected Cycle 2 wR= 0.01195 Using Levenberg-Marquardt: 0.00001 New wR= 0.01170 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.02794 with corrections 0.01072 Rint for all data: 0.02815 with corrections 0.01101 0 observations identified as outliers and rejected Cycle 3 wR= 0.01170 Using Levenberg-Marquardt: 0.00000 New wR= 0.01170 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.02794 with corrections 0.01073 Rint for all data: 0.02815 with corrections 0.01101 Final wR= 0.01170 Final frame scales: Min= 0.9673 Max= 1.1017 Final absorption correction factors: Amin= 0.9254 Amax= 1.0949 PROFFIT INFO: Inet (after scale3 abspack): min=1391.9063 max=2633161.7500 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=346.2763 max=45062.9258 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:2/24 125 reflections read from tmp file 42 reflections are rejected (1 as outliers, 41 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 28 9 Initial Chi^2= 0.18956 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.68851 Current error model SIG(F2)^2 = 87.01*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 59.91*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 59.91*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 2633162- 1390945 12 1894025.60 184.91 100.00 1347493- 834769 12 1013014.00 93.61 100.00 781385- 259077 12 486790.34 96.76 100.00 257873- 179814 12 213884.38 64.00 100.00 174758- 155071 12 162264.27 45.17 100.00 153287- 103938 12 126345.33 32.51 100.00 102117- 79946 12 90151.75 27.62 100.00 78933- 6523 12 51121.96 21.77 100.00 6483- 3572 12 5133.12 6.96 100.00 3485- 1392 17 2729.07 5.73 100.00 ------------------------------------------------------------------------------------ 2633162- 1392 125 388473.31 55.82 100.00 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 604766.89 127.23 100.00 1.32- 1.11 12 799504.44 95.78 100.00 1.09- 0.93 12 527444.40 72.78 100.00 0.92- 0.87 12 345557.39 53.64 100.00 0.85- 0.80 12 588228.37 64.91 100.00 0.80- 0.75 12 229278.67 33.71 100.00 0.73- 0.71 12 155001.65 28.65 100.00 0.71- 0.67 12 338684.18 40.19 100.00 0.67- 0.64 12 242139.49 31.42 100.00 0.64- 0.60 17 152464.56 23.38 100.00 ------------------------------------------------------------------------------------ 4.82- 0.60 125 388473.31 55.82 100.00 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 12 604766.89 127.23 100.00 4.82- 1.11 24 702135.66 111.50 100.00 4.82- 0.93 36 643905.24 98.60 100.00 4.82- 0.87 48 569318.28 87.36 100.00 4.82- 0.80 60 573100.30 82.87 100.00 4.82- 0.75 72 515796.69 74.68 100.00 4.82- 0.71 84 464254.54 68.10 100.00 4.82- 0.67 96 448558.25 64.61 100.00 4.82- 0.64 108 425622.83 60.92 100.00 4.82- 0.60 125 388473.31 55.82 100.00 ------------------------------------------------------------------------------------ 4.82- 0.60 125 388473.31 55.82 100.00 Scale applied to data: s=0.379771 (maximum obs:2633161.750,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.011; Rsigma 0.011: data 125 -> merged 78 With outlier rejection... Rint 0.011; Rsigma 0.011: data 124 -> merged 78 Rejected total: 1, method kkm 1, method Blessing 0 Completeness direct cell (a, b, c) = (8.358, 8.358, 8.358), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.597021, 4.825660 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 6 10 1.33 60.00 8 1.61 - 1.21 8 10 1.50 80.00 12 1.17 - 1.01 9 10 1.56 90.00 14 0.99 - 0.89 8 10 1.63 80.00 13 0.88 - 0.81 8 10 1.63 80.00 13 0.81 - 0.74 9 10 1.44 90.00 13 0.73 - 0.71 8 10 1.88 80.00 15 0.70 - 0.66 6 10 2.00 60.00 12 0.65 - 0.64 7 10 1.43 70.00 10 0.63 - 0.60 7 10 1.43 70.00 10 --------------------------------------------------------------- 5.92 - 0.60 76 100 1.58 76.00 120 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:05:11 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918870 5.905407 5.919111 59.8479 89.9883 60.0030 125 Reflections read from file xs1714a.hkl; mean (I/sigma) = 53.96 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 59 61 64 62 92 85 90 125 N (int>3sigma) = 0 58 61 63 62 91 84 89 122 Mean intensity = 0.0 13.7 5.7 13.1 13.2 10.9 16.4 14.2 13.9 Mean int/sigma = 0.0 50.3 50.1 50.5 51.7 50.3 61.2 57.2 54.0 Lattice type: P chosen Volume: 145.98 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.899 5.905 5.907 90.26 119.82 119.81 Niggli form: a.a = 34.794 b.b = 34.874 c.c = 34.892 b.c = -0.159 a.c = -17.326 a.b = -17.316 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.344 CUBIC F-lattice R(int) = 0.020 [ 31] Vol = 583.9 Cell: 8.372 8.370 8.334 90.13 89.99 90.00 Volume: 583.92 Matrix: 1.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.312 RHOMBOHEDRAL R-lattice R(int) = 0.218 [ 9] Vol = 437.9 Cell: 5.919 5.905 14.489 90.16 90.04 120.15 Volume: 437.94 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.312 RHOMBOHEDRAL R-lattice R(int) = 0.000 [ 0] Vol = 437.9 Trigonal Cell: 5.919 5.905 14.489 90.16 90.04 120.15 Volume: 437.94 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 3.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.126 TETRAGONAL I-lattice R(int) = 0.021 [ 4] Vol = 292.0 Cell: 5.919 5.919 8.334 89.92 89.90 90.01 Volume: 291.96 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.106 TETRAGONAL I-lattice R(int) = 0.021 [ 4] Vol = 292.0 Cell: 5.919 5.919 8.334 90.10 90.08 90.01 Volume: 291.96 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.129 ORTHORHOMBIC I-lattice R(int) = 0.035 [ 25] Vol = 292.0 Cell: 5.919 5.919 8.334 89.90 89.92 90.01 Volume: 291.96 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.109 ORTHORHOMBIC I-lattice R(int) = 0.031 [ 4] Vol = 292.0 Cell: 5.899 8.372 5.912 89.99 89.75 90.01 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.080 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 5.919 5.919 8.334 90.08 90.10 90.01 Volume: 291.96 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.203 MONOCLINIC I-lattice R(int) = 0.036 [ 3] Vol = 292.0 Cell: 5.899 5.912 8.372 90.01 90.01 90.25 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.019 MONOCLINIC I-lattice R(int) = 0.031 [ 4] Vol = 292.0 Cell: 5.899 8.372 5.912 89.99 90.25 89.99 Volume: 291.96 Matrix: 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.108 MONOCLINIC I-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 5.912 5.899 8.372 89.99 90.01 89.75 Volume: 291.96 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.275 MONOCLINIC C-lattice R(int) = 0.000 [ 0] Vol = 292.0 Cell: 10.237 5.905 5.907 90.26 125.15 89.77 Volume: 291.96 Matrix: 0.0000 -1.0000 2.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.0 Cell: 5.899 5.905 5.907 90.26 119.82 119.81 Volume: 145.98 Matrix: 0.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 61 0 85 82 125 N (int>3sigma) = 0 0 0 0 61 0 84 80 122 Mean intensity = 0.0 0.0 0.0 0.0 5.7 0.0 16.4 13.4 13.9 Mean int/sigma = 0.0 0.0 0.0 0.0 50.1 0.0 61.2 49.5 54.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.245 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 2 2 6 28 N I>3s 2 2 5 28 0.1 0.1 0.1 6.7 6.3 6.3 6.8 58.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.020 31 Fd-3m 1 1 227 C N N N N 37 2284 0.028 47 0kl, h0l, hk0, with too little data to consider diffraction symbol Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371571 8.369862 8.333516 90.1334 89.9855 89.9977 ZERR 1.00 0.002515 0.013964 0.033465 0.0284 0.1067 0.0215 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2624371- 253861 38 38 26 1.5 1085065.20 121.44 0.011 0.011 248317- 84552 45 45 26 1.7 144964.53 42.14 0.009 0.009 81827- 1392 42 41 26 1.6 19449.17 11.20 0.021 0.020 ------------------------------------------------------------------------------------------- 2624371- 1392 125 124 78 1.6 391558.85 56.21 0.011 0.011 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-0.93 36 36 26 1.4 643905.24 98.60 0.017 0.017 0.007 0.92-0.72 45 44 26 1.7 352110.74 47.26 0.007 0.007 0.013 0.71-0.60 44 44 26 1.7 224541.73 30.49 0.009 0.009 0.020 ------------------------------------------------------------------------------------------------------ inf-0.60 125 124 78 1.6 391558.85 56.21 0.011 0.011 0.011 inf-0.61 119 118 75 1.6 409236.20 58.34 0.011 0.011 0.011 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-0.93 36 35 26 74.3 1.4 643905.24 115.48 0.017 0.005 0.92-0.72 44 31 26 83.9 1.7 352110.74 66.23 0.007 0.008 0.71-0.60 44 37 26 70.3 1.7 224541.73 41.77 0.009 0.014 -------------------------------------------------------------------------------------------- inf-0.60 124 103 78 75.7 1.6 391558.85 71.85 0.011 0.008 inf-0.61 118 98 75 76.5 1.6 409236.20 74.52 0.011 0.008 ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:12:34 2018) ID: 2932; threads 39; handles 876; mem 517540.00 (1237820.00)kB; time: 1w 4d 22h 18m 5s MEMORY INFO: Memory PF:243.0, Ph:421.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:505.5,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:245.0, Ph:421.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.3,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:12:34 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000045 0.000108 0.000080 ) -0.068858 -0.065594 -0.010716 ( 0.000068 0.000163 0.000122 ) 0.109112 -0.153091 0.115835 ( 0.000073 0.000175 0.000131 ) 5.91502 ( 0.00694 ) 5.91640 ( 0.00720 ) 5.92265 ( 0.00472 ) 60.05206 ( 0.10391 ) 89.98756 ( 0.07838 ) 60.01743 ( 0.12498 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:12:34 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000045 0.000108 0.000080 ) -0.068858 -0.065594 -0.010716 ( 0.000068 0.000163 0.000122 ) 0.109112 -0.153091 0.115835 ( 0.000073 0.000175 0.000131 ) M - matrix: 0.021568 -0.014452 0.007238 ( 0.000019 0.000026 0.000020 ) -0.014452 0.028978 -0.014519 ( 0.000026 0.000059 0.000031 ) 0.007238 -0.014519 0.021634 ( 0.000020 0.000031 0.000034 ) unit cell: 5.915(7) 5.916(7) 5.923(5) 60.05(10) 89.99(8) 60.02(12) V = 146.7(2) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb PROFFITPEAK info: 767 peaks in the peak location table UB fit with 291 obs out of 320 (total:321,skipped:1) (90.94%) UB - matrix: -0.070169 0.030768 0.088701 ( 0.000085 0.000166 0.000105 ) -0.067992 -0.066227 -0.010643 ( 0.000102 0.000200 0.000126 ) 0.109089 -0.152792 0.116121 ( 0.000157 0.000308 0.000195 ) M - matrix: 0.021447 -0.014324 0.007167 ( 0.000039 0.000046 0.000031 ) -0.014324 0.028678 -0.014308 ( 0.000046 0.000098 0.000050 ) 0.007167 -0.014308 0.021465 ( 0.000031 0.000050 0.000049 ) unit cell: 5.933(9) 5.920(10) 5.926(7) 60.08(14) 90.08(11) 60.01(17) V = 147.3(3) UB fit with 291 obs out of 320 (total:321,skipped:1) (90.94%) UB - matrix: -0.070169 0.030768 0.088701 ( 0.000085 0.000166 0.000105 ) -0.067992 -0.066227 -0.010643 ( 0.000102 0.000200 0.000126 ) 0.109089 -0.152792 0.116121 ( 0.000157 0.000308 0.000195 ) M - matrix: 0.021447 -0.014324 0.007167 ( 0.000039 0.000046 0.000031 ) -0.014324 0.028678 -0.014308 ( 0.000046 0.000098 0.000050 ) 0.007167 -0.014308 0.021465 ( 0.000031 0.000050 0.000049 ) unit cell: 5.933(9) 5.920(10) 5.926(7) 60.08(14) 90.08(11) 60.01(17) V = 147.3(3) OTKP changes: 50 1 1 1 UB - matrix: -0.070194 0.030708 0.088559 ( 0.000091 0.000179 0.000113 ) -0.068135 -0.065966 -0.010635 ( 0.000095 0.000186 0.000118 ) 0.109019 -0.152889 0.116081 ( 0.000142 0.000279 0.000176 ) M - matrix: 0.021455 -0.014329 0.007163 ( 0.000036 0.000042 0.000029 ) -0.014329 0.028670 -0.014327 ( 0.000042 0.000089 0.000046 ) 0.007163 -0.014327 0.021431 ( 0.000029 0.000046 0.000046 ) UB fit with 292 obs out of 320 (total:321,skipped:1) (91.25%) unit cell: 5.933(9) 5.928(9) 5.937(7) 59.97(14) 90.01(11) 59.99(16) V = 147.6(3) UB fit with 292 obs out of 320 (total:321,skipped:1) (91.25%) UB - matrix: -0.070194 0.030708 0.088559 ( 0.000091 0.000179 0.000113 ) -0.068135 -0.065966 -0.010635 ( 0.000095 0.000186 0.000118 ) 0.109019 -0.152889 0.116081 ( 0.000142 0.000279 0.000176 ) M - matrix: 0.021455 -0.014329 0.007163 ( 0.000036 0.000042 0.000029 ) -0.014329 0.028670 -0.014327 ( 0.000042 0.000089 0.000046 ) 0.007163 -0.014327 0.021431 ( 0.000029 0.000046 0.000046 ) unit cell: 5.933(9) 5.928(9) 5.937(7) 59.97(14) 90.01(11) 59.99(16) V = 147.6(3) OTKP changes: 50 1 1 1 UB - matrix: -0.070194 0.030757 0.088594 ( 0.000091 0.000179 0.000113 ) -0.068100 -0.066033 -0.010524 ( 0.000095 0.000186 0.000117 ) 0.109118 -0.152957 0.116099 ( 0.000142 0.000279 0.000176 ) M - matrix: 0.021471 -0.014352 0.007166 ( 0.000036 0.000042 0.000029 ) -0.014352 0.028702 -0.014338 ( 0.000042 0.000089 0.000046 ) 0.007166 -0.014338 0.021439 ( 0.000029 0.000046 0.000046 ) UB fit with 293 obs out of 320 (total:321,skipped:1) (91.56%) unit cell: 5.933(9) 5.927(9) 5.936(7) 59.97(14) 89.99(11) 59.96(16) V = 147.5(3) 321 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Run 1 Omega scan: (-107.000 - -57.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.874) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070194 0.030757 0.088594 ( 0.000091 0.000179 0.000113 ) -0.068100 -0.066033 -0.010524 ( 0.000095 0.000186 0.000117 ) 0.109118 -0.152957 0.116099 ( 0.000142 0.000279 0.000176 ) M - matrix: 0.021472 -0.014352 0.007166 ( 0.000036 0.000042 0.000029 ) -0.014352 0.028702 -0.014338 ( 0.000042 0.000089 0.000046 ) 0.007166 -0.014338 0.021439 ( 0.000029 0.000046 0.000046 ) UB fit with 293 obs out of 320 (total:321,skipped:1) (91.56%) unit cell: 5.933(9) 5.927(9) 5.936(7) 59.97(14) 89.99(11) 59.96(16) V = 147.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 293 obs out of 320 (total:321,skipped:1) (91.56%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb 4 of 198 peaks identified as outliers and rejected 194 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 194 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 194 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.72- 1.41 | 19 | 0.950 ( 0.158) | 1.162 ( 0.536) | 1.225 ( 0.812) | 1.38- 1.12 | 19 | 1.053 ( 0.107) | 1.162 ( 0.352) | 1.306 ( 0.512) | 1.12- 0.97 | 19 | 1.092 ( 0.107) | 1.110 ( 0.120) | 1.055 ( 0.412) | 0.97- 0.88 | 19 | 1.084 ( 0.106) | 1.078 ( 0.141) | 1.034 ( 0.442) | 0.87- 0.81 | 19 | 1.145 ( 0.095) | 1.018 ( 0.097) | 1.638 ( 0.420) | 0.81- 0.75 | 19 | 1.123 ( 0.093) | 0.999 ( 0.145) | 1.506 ( 0.542) | 0.75- 0.71 | 19 | 1.155 ( 0.073) | 0.972 ( 0.124) | 1.460 ( 0.535) | 0.71- 0.67 | 19 | 1.129 ( 0.057) | 0.890 ( 0.074) | 1.451 ( 0.561) | 0.67- 0.64 | 19 | 1.109 ( 0.047) | 0.870 ( 0.072) | 1.373 ( 0.548) | 0.63- 0.59 | 23 | 1.103 ( 0.065) | 0.827 ( 0.049) | 1.357 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.72- 0.59 | 194 | 1.094 ( 0.110) | 1.005 ( 0.251) | 1.341 ( 0.577) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 194 obs out of 194 (total:194,skipped:0) (100.00%) UB - matrix: -0.070100 0.030364 0.088858 ( 0.000035 0.000062 0.000037 ) -0.068552 -0.065564 -0.010718 ( 0.000054 0.000095 0.000057 ) 0.109303 -0.153179 0.115939 ( 0.000044 0.000078 0.000047 ) M - matrix: 0.021561 -0.014377 0.007178 ( 0.000013 0.000014 0.000009 ) -0.014377 0.028684 -0.014359 ( 0.000014 0.000027 0.000013 ) 0.007178 -0.014359 0.021452 ( 0.000009 0.000013 0.000013 ) unit cell: 5.920(4) 5.933(4) 5.939(2) 59.89(6) 89.93(4) 59.95(7) V = 147.24(14) OTKP changes: 194 1 1 1 UB - matrix: -0.070134 0.030606 0.088877 ( 0.000024 0.000042 0.000026 ) -0.068450 -0.065874 -0.010779 ( 0.000046 0.000081 0.000049 ) 0.109192 -0.153277 0.116233 ( 0.000043 0.000076 0.000046 ) M - matrix: 0.021527 -0.014374 0.007196 ( 0.000012 0.000013 0.000008 ) -0.014374 0.028770 -0.014386 ( 0.000013 0.000026 0.000012 ) 0.007196 -0.014386 0.021525 ( 0.000008 0.000012 0.000012 ) UB fit with 194 obs out of 194 (total:194,skipped:0) (100.00%) unit cell: 5.922(3) 5.917(4) 5.9248(19) 59.97(5) 90.04(3) 60.02(6) V = 146.73(11) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -57.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.890) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070134 0.030606 0.088877 ( 0.000024 0.000042 0.000026 ) -0.068450 -0.065874 -0.010779 ( 0.000046 0.000081 0.000049 ) 0.109192 -0.153277 0.116233 ( 0.000043 0.000076 0.000046 ) M - matrix: 0.021527 -0.014374 0.007196 ( 0.000012 0.000013 0.000008 ) -0.014374 0.028770 -0.014386 ( 0.000013 0.000026 0.000012 ) 0.007196 -0.014386 0.021525 ( 0.000008 0.000012 0.000012 ) UB fit with 194 obs out of 194 (total:194,skipped:0) (100.00%) unit cell: 5.922(3) 5.917(4) 5.9248(19) 59.97(5) 90.04(3) 60.02(6) V = 146.73(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 194 obs out of 194 (total:194,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb 4 of 194 peaks identified as outliers and rejected 190 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 190 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 190 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 19 | 0.957 ( 0.159) | 1.186 ( 0.590) | 1.259 ( 0.814) | 1.32- 1.09 | 19 | 1.075 ( 0.093) | 1.092 ( 0.092) | 1.187 ( 0.471) | 1.09- 0.94 | 19 | 1.094 ( 0.109) | 1.126 ( 0.143) | 1.030 ( 0.424) | 0.94- 0.85 | 19 | 1.088 ( 0.107) | 1.048 ( 0.127) | 1.147 ( 0.473) | 0.84- 0.81 | 19 | 1.171 ( 0.067) | 1.047 ( 0.097) | 1.603 ( 0.436) | 0.81- 0.73 | 19 | 1.105 ( 0.101) | 0.978 ( 0.136) | 1.444 ( 0.540) | 0.73- 0.71 | 19 | 1.150 ( 0.066) | 0.946 ( 0.111) | 1.518 ( 0.483) | 0.70- 0.67 | 19 | 1.131 ( 0.051) | 0.892 ( 0.073) | 1.342 ( 0.501) | 0.66- 0.63 | 19 | 1.116 ( 0.043) | 0.886 ( 0.078) | 1.432 ( 0.561) | 0.63- 0.59 | 19 | 1.090 ( 0.066) | 0.810 ( 0.033) | 1.304 ( 0.547) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 190 | 1.098 ( 0.107) | 1.001 ( 0.239) | 1.327 ( 0.561) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-15.0 | 19 | 1.137 ( 0.049) | 1.174 ( 0.100) | 1.137 ( 0.537) | 15.1-19.3 | 19 | 1.139 ( 0.084) | 1.196 ( 0.331) | 1.467 ( 0.683) | 19.4-23.8 | 19 | 1.158 ( 0.081) | 1.086 ( 0.083) | 1.467 ( 0.517) | 24.3-27.8 | 19 | 1.129 ( 0.111) | 1.180 ( 0.453) | 1.521 ( 0.531) | 28.5-30.9 | 19 | 1.098 ( 0.094) | 0.989 ( 0.110) | 1.400 ( 0.511) | 31.0-34.2 | 19 | 1.112 ( 0.085) | 0.931 ( 0.098) | 1.317 ( 0.480) | 34.6-37.0 | 19 | 1.051 ( 0.097) | 0.893 ( 0.087) | 1.317 ( 0.605) | 37.0-39.4 | 19 | 1.084 ( 0.095) | 0.899 ( 0.069) | 1.313 ( 0.481) | 39.6-42.7 | 19 | 1.008 ( 0.124) | 0.842 ( 0.101) | 1.101 ( 0.486) | 42.7-49.3 | 19 | 1.061 ( 0.130) | 0.822 ( 0.067) | 1.228 ( 0.585) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.3 | 190 | 1.098 ( 0.107) | 1.001 ( 0.239) | 1.327 ( 0.561) | Fitted profile normalization line parameters e1 dimension: a=-0.0013 b=1.08 e2 dimension: a=-0.0102 b=1.27 e3 dimension: a=0.0063 b=0.95 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7487 lp-corr: 4093 Maximum peak integral for reflections I/sig<= 100 - raw: 484671 lp-corr: 697765 Maximum peak integral for reflections I/sig<= 10000 - raw: 5467306 lp-corr: 2106075 PROFFITPEAK - Finished at Tue Mar 27 13:12:38 2018 PROFFITMAIN - Started at Tue Mar 27 13:12:38 2018 OTKP changes: 190 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 190 1 1 1 UB - matrix: -0.070208 0.030705 0.088936 ( 0.000023 0.000041 0.000024 ) -0.068472 -0.065913 -0.010706 ( 0.000041 0.000071 0.000043 ) 0.109286 -0.153391 0.116312 ( 0.000041 0.000072 0.000043 ) M - matrix: 0.021561 -0.014406 0.007200 ( 0.000011 0.000012 0.000008 ) -0.014406 0.028816 -0.014405 ( 0.000012 0.000024 0.000012 ) 0.007200 -0.014405 0.021553 ( 0.000008 0.000012 0.000011 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 5.919(3) 5.914(3) 5.9207(17) 59.97(4) 90.00(3) 59.97(5) V = 146.44(10) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -57.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.823) HKL list info: 433 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070208 0.030705 0.088936 ( 0.000023 0.000041 0.000024 ) -0.068472 -0.065913 -0.010706 ( 0.000041 0.000071 0.000043 ) 0.109286 -0.153391 0.116312 ( 0.000041 0.000072 0.000043 ) M - matrix: 0.021561 -0.014406 0.007200 ( 0.000011 0.000012 0.000008 ) -0.014406 0.028816 -0.014405 ( 0.000012 0.000024 0.000012 ) 0.007200 -0.014405 0.021553 ( 0.000008 0.000012 0.000011 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 5.919(3) 5.914(3) 5.9207(17) 59.97(4) 90.00(3) 59.97(5) V = 146.44(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070208 0.030705 0.088936 ( 0.000023 0.000041 0.000024 ) -0.068472 -0.065913 -0.010706 ( 0.000041 0.000071 0.000043 ) 0.109286 -0.153391 0.116312 ( 0.000041 0.000072 0.000043 ) M - matrix: 0.021561 -0.014406 0.007200 ( 0.000011 0.000012 0.000008 ) -0.014406 0.028816 -0.014405 ( 0.000012 0.000024 0.000012 ) 0.007200 -0.014405 0.021553 ( 0.000008 0.000012 0.000011 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 5.919(3) 5.914(3) 5.9207(17) 59.97(4) 90.00(3) 59.97(5) V = 146.44(10) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070208 0.030705 0.088936 ( 0.000023 0.000041 0.000024 ) -0.068472 -0.065913 -0.010706 ( 0.000041 0.000071 0.000043 ) 0.109286 -0.153391 0.116312 ( 0.000041 0.000072 0.000043 ) M - matrix: 0.021561 -0.014406 0.007200 ( 0.000011 0.000012 0.000008 ) -0.014406 0.028816 -0.014405 ( 0.000012 0.000024 0.000012 ) 0.007200 -0.014405 0.021553 ( 0.000008 0.000012 0.000011 ) UB fit with 190 obs out of 190 (total:190,skipped:0) (100.00%) unit cell: 5.919(3) 5.914(3) 5.9207(17) 59.97(4) 90.00(3) 59.97(5) V = 146.44(10) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 12 reflections under beam stop or inside a detector rejection region 1 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof 279 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:12:39 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -57.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.823) PROFFIT INFO: signal sum: min=137.0000 max=12258056.0000 PROFFIT INFO: signal sum lp corr: min=699.9696 max=2624425.8269 PROFFIT INFO: background sum: min=1646.0000 max=7626.0000 PROFFIT INFO: background sum sig2: min=702.0000 max=5785.0000 PROFFIT INFO: num of signal pixels: min=63 max=484 PROFFIT INFO: Inet: min=1119.9514 max=4199081.5000 PROFFIT INFO: sig(Inet): min=183.0573 max=47089.1953 PROFFIT INFO: Inet/sig(Inet): min=1.05 max=230.83 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 3 10 31 65 69 106 180 247 279 Percent 0.0 0.0 1.1 3.6 11.1 23.3 24.7 38.0 64.5 88.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 279 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 279 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4199082- 1272631 27 2032186.92 137.79 100.00 1270130- 807467 27 1017948.55 111.78 100.00 802221- 317720 27 497649.51 104.25 100.00 316222- 198319 27 227523.94 69.13 100.00 197139- 155270 27 174079.19 60.19 100.00 155157- 107870 27 133066.75 38.85 100.00 107538- 85319 27 97462.88 32.77 100.00 83752- 6470 27 53072.84 22.95 100.00 6428- 3523 27 4856.64 5.14 92.59 3496- 1120 36 2707.51 4.24 77.78 ------------------------------------------------------------------------------------ 4199082- 1120 279 410463.60 56.95 96.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.15 27 783531.09 92.97 100.00 1.12- 0.90 27 482561.86 58.50 100.00 0.90- 0.78 27 694922.20 89.75 100.00 0.78- 0.72 27 455361.37 72.06 96.30 0.72- 0.65 27 443858.74 66.51 100.00 0.65- 0.61 27 253440.09 40.77 96.30 0.61- 0.58 27 369838.71 50.74 96.30 0.57- 0.55 27 175088.39 30.52 92.59 0.55- 0.52 27 333684.61 47.61 92.59 0.52- 0.42 36 186877.63 29.33 91.67 ------------------------------------------------------------------------------------ 5.26- 0.42 279 410463.60 56.95 96.42 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:12:39 2018 Sorting 279 observations 63 unique observations with > 7.00 F2/sig(F2) 279 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Maximum number of 63 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 279 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 216 observations > 7.00 F2/sig(F2) 216 observations in 1 runs Run # start # end # total # 1 0 48 49 Total number of frames 49 Removing 'redundancy=1' reflections Average redundancy: 2.2 (Out of 216 removed 106 = 110, unique = 49) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 110 observations in 1 runs Run # start # end # total # 1 0 48 49 Total number of frames 49 Frame #14 of 49 skipped from refinement Frame #15 of 49 skipped from refinement Frame #23 of 49 skipped from refinement Frame #30 of 49 skipped from refinement Frame #47 of 49 skipped from refinement 5 frames need to be skipped from refinement, because of missing redundant and/or observable data 49 unique data precomputed (should be 49) 49 unique data with 110 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.2 (Out of 110 removed 0 = 110, unique = 49) 49 unique data precomputed (should be 49) 49 unique data with 110 observations RMS deviation of equivalent data = 0.58043 Rint = 0.43940 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.43940, wR= 2.64122 Trying model 1 (ne=2, no=0)... Results: Rint= 0.37981, wR= 1.40170, Acormin=-0.255, Acormax=0.793, Acor_av=0.243 F test: Probability=0.782, F= 1.229 Trying model 2 (ne=2, no=1)... Results: Rint= 0.68150, wR= 2.60913, Acormin=-0.277, Acormax=0.366, Acor_av=-0.025 F test: Probability=0.000, F= 0.361 Trying model 3 (ne=4, no=0)... Results: Rint= 0.23931, wR= 0.45582, Acormin=-0.066, Acormax=0.699, Acor_av=0.125 F test: Probability=1.000, F= 2.597 Trying model 4 (ne=4, no=1)... Results: Rint= 0.31343, wR= 0.61629, Acormin=-0.071, Acormax=0.164, Acor_av=0.041 F test: Probability=0.887, F= 1.418 Trying model 5 (ne=4, no=3)... Results: Rint= 0.17006, wR= 0.41264, Acormin=-0.031, Acormax=0.275, Acor_av=0.052 F test: Probability=1.000, F= 4.050 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.67160 There are 44 active scales (one needs to be fixed) Refinement control: frame scale #16 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 48 pars with 1176 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.58043 Using Levenberg-Marquardt: 0.00010 New wR= 0.54261 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.68946 Rint for all data: 0.67160 with corrections 0.82873 0 observations identified as outliers and rejected Cycle 2 wR= 0.54480 Using Levenberg-Marquardt: 0.00001 New wR= 0.50303 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.47134 Rint for all data: 0.67160 with corrections 0.70458 0 observations identified as outliers and rejected Cycle 3 wR= 0.50321 Using Levenberg-Marquardt: 0.00000 New wR= 0.78825 Using Levenberg-Marquardt: 0.00001 New wR= 0.78819 Using Levenberg-Marquardt: 0.00010 New wR= 0.78763 Using Levenberg-Marquardt: 0.00100 New wR= 0.78190 Using Levenberg-Marquardt: 0.01000 New wR= 0.73230 Using Levenberg-Marquardt: 0.10000 New wR= 0.60309 Using Levenberg-Marquardt: 1.00000 New wR= 0.46173 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.44376 Rint for all data: 0.67160 with corrections 0.67594 0 observations identified as outliers and rejected Cycle 4 wR= 0.46078 Using Levenberg-Marquardt: 0.10000 New wR= 0.43662 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.43779 Rint for all data: 0.67160 with corrections 0.67091 0 observations identified as outliers and rejected Cycle 5 wR= 0.43486 Using Levenberg-Marquardt: 0.01000 New wR= 0.46762 Using Levenberg-Marquardt: 0.10000 New wR= 0.42325 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.43153 Rint for all data: 0.67160 with corrections 0.66769 0 observations identified as outliers and rejected Final wR= 0.42325 Final frame scales: Min= 0.2919 Max= 7.1854 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time with different frame scales initialization There are 44 active scales (one needs to be fixed) Refinement control: frame scale #16 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 43 pars with 946 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.95479 Using Levenberg-Marquardt: 0.00010 New wR= 0.62000 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.63689 Rint for all data: 0.67160 with corrections 0.76278 0 observations identified as outliers and rejected Cycle 2 wR= 0.61380 Using Levenberg-Marquardt: 0.00001 New wR= 0.54242 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.46489 Rint for all data: 0.67160 with corrections 0.67227 0 observations identified as outliers and rejected Cycle 3 wR= 0.53457 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.49103 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.35519 Rint for all data: 0.67160 with corrections 0.62733 0 observations identified as outliers and rejected Cycle 4 wR= 0.48567 Using Levenberg-Marquardt: 0.00100 New wR= 0.49312 Using Levenberg-Marquardt: 0.01000 New wR= 0.48448 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.33817 Rint for all data: 0.67160 with corrections 0.61829 0 observations identified as outliers and rejected Cycle 5 wR= 0.47797 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.48708 Using Levenberg-Marquardt: 0.10000 New wR= 0.46846 There are 5 clusters with unrefined scales (size 1-3) Rint for refined data: 0.43940 with corrections 0.30984 Rint for all data: 0.67160 with corrections 0.60926 0 observations identified as outliers and rejected Final wR= 0.46846 Final frame scales: Min= 7.7315 Max=143.1034 Frame scales outside specified range! Trying one more time after skipping bad frame scales SCALE3 WARNING: No scale needs refinement Frame scaling turned off SCALE3 ERROR: No parameters to be refined! ! SCALE3 WARNING: Frame scaling turned off due to lack of scales requiring refinement Can't fit requested scale/empirical absorption model (pTmpToScale3AbspackHKL) ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:1/50 279 reflections read from tmp file 226 reflections are rejected (114 as outliers, 112 as groups of 1 refl) Redundancy: 1 2 3+ Number of groups: 0 25 1 Initial Chi^2= 0.48171 Cycle 1, Chi^2= 0.98855 Current error model SIG(F2)^2 = 44.00*I_RAW + 26.52*I_BACK+(0.06050*)^2 Cycle 2, Chi^2= 1.00330 Current error model SIG(F2)^2 = 65.72*I_RAW + 17.64*I_BACK+(0.05650*)^2 Cycle 3, Chi^2= 1.00390 Current error model SIG(F2)^2 = 81.74*I_RAW + 13.93*I_BACK+(0.05351*)^2 Cycle 4, Chi^2= 1.00415 Current error model SIG(F2)^2 = 95.91*I_RAW + 11.09*I_BACK+(0.05083*)^2 Cycle 5, Chi^2= 1.00424 Current error model SIG(F2)^2 = 109.73*I_RAW + 8.62*I_BACK+(0.04816*)^2 Cycle 6, Chi^2= 1.00457 Current error model SIG(F2)^2 = 124.39*I_RAW + 6.10*I_BACK+(0.04526*)^2 Cycle 7, Chi^2= 1.00490 Current error model SIG(F2)^2 = 140.94*I_RAW + 3.40*I_BACK+(0.04188*)^2 Cycle 8, Chi^2= 1.00529 Current error model SIG(F2)^2 = 160.64*I_RAW + 0.24*I_BACK+(0.03764*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 9, Chi^2= 0.98623 Current error model SIG(F2)^2 = 184.96*I_RAW + 0.00*I_BACK+(0.03195*)^2 Cycle 10, Chi^2= 0.99741 Current error model SIG(F2)^2 = 200.38*I_RAW + 0.00*I_BACK+(0.02615*)^2 Final Chi^2= 0.99741 Final error model SIG(F2)^2 = 200.38*I_RAW + 0.00*I_BACK+(0.02615*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4199082- 1272631 27 2032186.92 71.81 100.00 1270130- 807467 27 1017948.55 40.34 100.00 802221- 317720 27 497649.51 38.49 100.00 316222- 198319 27 227523.94 26.13 100.00 197139- 155270 27 174079.19 22.59 100.00 155157- 107870 27 133066.75 16.43 100.00 107538- 85319 27 97462.88 14.35 100.00 83752- 6470 27 53072.84 10.57 100.00 6428- 3523 27 4856.64 3.60 66.67 3496- 1120 36 2707.51 3.26 55.56 ------------------------------------------------------------------------------------ 4199082- 1120 279 410463.60 24.06 91.04 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.15 27 783531.09 43.98 100.00 1.12- 0.90 27 482561.86 33.86 88.89 0.90- 0.78 27 694922.20 35.86 96.30 0.78- 0.72 27 455361.37 26.89 96.30 0.72- 0.65 27 443858.74 22.70 100.00 0.65- 0.61 27 253440.09 18.12 85.19 0.61- 0.58 27 369838.71 18.40 88.89 0.57- 0.55 27 175088.39 13.77 81.48 0.55- 0.52 27 333684.61 17.71 92.59 0.52- 0.42 36 186877.63 13.02 83.33 ------------------------------------------------------------------------------------ 5.26- 0.42 279 410463.60 24.06 91.04 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.15 27 783531.09 43.98 100.00 5.26- 0.90 54 633046.47 38.92 94.44 5.26- 0.78 81 653671.72 37.90 95.06 5.26- 0.72 108 604094.13 35.15 95.37 5.26- 0.65 135 572047.05 32.66 96.30 5.26- 0.61 162 518945.89 30.24 94.44 5.26- 0.58 189 497644.86 28.54 93.65 5.26- 0.55 216 457325.31 26.70 92.13 5.26- 0.52 243 443587.45 25.70 92.18 5.26- 0.42 279 410463.60 24.06 91.04 ------------------------------------------------------------------------------------ 5.26- 0.42 279 410463.60 24.06 91.04 Scale applied to data: s=0.238147 (maximum obs:4199081.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.672; Rsigma 0.028: data 279 -> merged 183 With outlier rejection... Rint 0.489; Rsigma 0.029: data 263 -> merged 183 Rejected total: 16, method kkm 16, method Blessing 0 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.424741, 5.270892 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 11 15 1.18 73.33 13 1.46 - 1.12 8 15 1.50 53.33 12 1.08 - 0.96 7 15 1.86 46.67 13 0.96 - 0.86 11 15 1.64 73.33 18 0.86 - 0.79 8 15 1.75 53.33 14 0.79 - 0.73 9 15 1.89 60.00 17 0.73 - 0.69 10 15 1.50 66.67 15 0.69 - 0.65 13 15 1.54 86.67 20 0.65 - 0.63 8 15 1.50 53.33 12 0.63 - 0.60 18 21 1.33 85.71 24 --------------------------------------------------------------- 5.92 - 0.60 103 156 1.53 66.03 158 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:12:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919271 5.914130 5.920691 59.9685 89.9961 59.9738 263 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 126 133 133 131 196 177 183 263 N (int>3sigma) = 0 113 133 120 117 183 161 165 239 Mean intensity = 0.0 86.5 40.8 86.3 93.1 70.9 103.1 101.5 96.1 Mean int/sigma = 0.0 21.5 21.2 22.2 24.7 21.6 23.8 24.4 23.3 Lattice type: P chosen Volume: 146.44 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.914 5.914 5.915 90.10 119.93 119.94 Niggli form: a.a = 34.977 b.b = 34.980 c.c = 34.982 b.c = -0.063 a.c = -17.452 a.b = -17.459 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.035 [ 123] Vol = 585.7 Cell: 8.372 8.372 8.357 90.01 90.00 90.01 Volume: 585.75 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.090 RHOMBOHEDRAL R-lattice R(int) = 0.065 [ 41] Vol = 439.3 Cell: 5.919 5.914 14.494 90.09 90.01 120.03 Volume: 439.31 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.090 RHOMBOHEDRAL R-lattice R(int) = 0.093 [ 3] Vol = 439.3 Trigonal Cell: 5.919 5.914 14.494 90.09 90.01 120.03 Volume: 439.31 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.008 TETRAGONAL I-lattice R(int) = 0.037 [ 72] Vol = 292.9 Cell: 5.921 5.919 8.357 89.99 89.99 90.00 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.014 TETRAGONAL I-lattice R(int) = 0.037 [ 72] Vol = 292.9 Cell: 5.919 5.921 8.357 90.01 90.01 90.00 Volume: 292.87 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.007 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 120] Vol = 292.9 Cell: 5.919 5.921 8.357 89.99 89.99 90.00 Volume: 292.87 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.021 [ 31] Vol = 292.9 Cell: 5.914 8.372 5.915 89.99 89.89 89.99 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.004 MONOCLINIC I-lattice R(int) = 0.029 [ 72] Vol = 292.9 Cell: 5.921 5.919 8.357 90.01 90.01 90.00 Volume: 292.87 Matrix: 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.078 MONOCLINIC I-lattice R(int) = 0.020 [ 27] Vol = 292.9 Cell: 5.914 5.915 8.372 90.01 90.01 89.89 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.008 MONOCLINIC I-lattice R(int) = 0.049 [ 4] Vol = 292.9 Cell: 5.914 8.372 5.915 89.99 90.11 90.01 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.046 MONOCLINIC I-lattice R(int) = 0.002 [ 1] Vol = 292.9 Cell: 5.915 5.914 8.372 89.99 90.01 90.11 Volume: 292.87 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.080 MONOCLINIC C-lattice R(int) = 0.036 [ 8] Vol = 292.9 Cell: 10.249 5.914 5.915 90.10 125.23 89.94 Volume: 292.87 Matrix:-1.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.4 Cell: 5.914 5.914 5.915 90.10 119.93 119.94 Volume: 146.44 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 133 0 179 175 263 N (int>3sigma) = 0 0 0 0 133 0 166 162 239 Mean intensity = 0.0 0.0 0.0 0.0 40.8 0.0 93.0 102.2 96.1 Mean int/sigma = 0.0 0.0 0.0 0.0 21.2 0.0 22.6 24.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.271 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 4 4 22 60 N I>3s 4 4 19 60 1.0 1.0 1.0 47.3 5.8 5.8 4.1 24.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 119 Fd-3m 1 1 227 C N N N N 37 2284 0.033 152 0kl, h0l, hhl, with too little data to consider diffraction symbol Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371833 8.372402 8.356829 90.0106 89.9977 90.0137 ZERR 1.00 0.005665 0.001075 0.014481 0.0450 0.0168 0.0123 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4199082- 896720 39 37 26 1.4 1520266.41 47.63 0.387 0.387 869841- 442189 48 41 26 1.6 581207.66 31.69 0.752 0.752 415048- 190757 50 46 26 1.8 303341.45 27.58 0.535 0.544 188377- 120999 41 38 26 1.5 164176.52 19.76 0.124 0.124 120184- 92573 33 33 26 1.3 102984.26 15.17 0.433 0.433 92554- 5707 35 35 26 1.3 66804.02 12.32 0.370 0.370 5628- 1381 33 33 27 1.2 3214.43 3.20 0.166 0.166 ------------------------------------------------------------------------------------------- 4199082- 1381 279 263 183 1.4 403477.12 23.26 0.489 0.491 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-0.98 46 38 26 1.5 717256.15 43.30 0.283 0.283 0.018 0.96-0.75 49 45 26 1.7 549969.03 28.36 0.711 0.721 0.025 0.75-0.65 46 42 27 1.6 435519.20 23.53 0.321 0.321 0.030 0.65-0.60 36 36 26 1.4 347156.65 19.41 0.635 0.635 0.033 0.59-0.56 36 36 27 1.3 188356.15 14.38 0.681 0.681 0.044 0.55-0.51 38 38 28 1.4 282672.04 15.81 0.504 0.504 0.041 0.51-0.42 28 28 23 1.2 207083.50 13.97 0.874 0.874 0.043 ------------------------------------------------------------------------------------------------------ inf-0.42 279 263 183 1.4 403477.12 23.26 0.489 0.491 0.029 inf-0.60 174 158 103 1.5 517072.73 28.75 0.460 0.461 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-0.98 38 44 26 59.1 1.5 717256.15 58.93 0.283 0.009 0.96-0.75 45 42 26 61.9 1.7 549969.03 44.00 0.711 0.017 0.75-0.65 42 40 27 67.5 1.6 435519.20 33.38 0.321 0.021 0.65-0.60 36 32 26 81.3 1.4 347156.65 27.63 0.635 0.023 0.59-0.56 36 38 27 71.1 1.3 188356.15 19.21 0.681 0.032 0.55-0.51 38 45 28 62.2 1.4 282672.04 20.39 0.504 0.030 0.51-0.42 28 165 23 13.9 1.2 207083.50 18.45 0.874 0.030 -------------------------------------------------------------------------------------------- inf-0.42 263 406 183 45.1 1.4 403477.12 32.70 0.489 0.019 inf-0.60 158 156 103 66.0 1.5 517072.73 41.35 0.460 0.016 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 1.0 -1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 1.0 -1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: 0.079572 -0.024717 -0.015352 ( 0.000010 0.000010 0.000020 ) 0.028883 0.072546 0.032957 ( 0.000017 0.000018 0.000035 ) 0.003513 -0.036104 0.076696 ( 0.000017 0.000018 0.000036 ) M - matrix: 0.007178 0.000002 -0.000000 ( 0.000002 0.000002 0.000002 ) 0.000002 0.007177 0.000001 ( 0.000002 0.000003 0.000003 ) -0.000000 0.000001 0.007204 ( 0.000002 0.000003 0.000006 ) Constraint UB - matrix: 0.079572 -0.024717 -0.015352 ( 0.000010 0.000010 0.000020 ) 0.028883 0.072546 0.032957 ( 0.000017 0.000018 0.000035 ) 0.003513 -0.036104 0.076696 ( 0.000017 0.000018 0.000036 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3718(12) 8.372(2) 8.357(3) 90.01(3) 89.998(18) 90.014(16) V = 585.8(3) unit cell: 8.3670(4) 8.3670(4) 8.3670(4) 90.0 90.0 90.0 V = 585.75(5) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -57.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.823) PROFFIT INFO: signal sum: min=137.0000 max=12258056.0000 PROFFIT INFO: signal sum lp corr: min=699.9696 max=2624425.8269 PROFFIT INFO: background sum: min=1646.0000 max=7626.0000 PROFFIT INFO: background sum sig2: min=702.0000 max=5785.0000 PROFFIT INFO: num of signal pixels: min=63 max=484 PROFFIT INFO: Inet: min=1119.9514 max=4199081.5000 PROFFIT INFO: sig(Inet): min=183.0573 max=47089.1953 PROFFIT INFO: Inet/sig(Inet): min=1.05 max=230.83 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 6 20 62 130 138 212 360 494 558 Percent 0.0 0.0 1.1 3.6 11.1 23.3 24.7 38.0 64.5 88.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 279 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 279 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4199082- 1272631 27 2032186.92 137.79 100.00 1270130- 807467 27 1017948.55 111.78 100.00 802221- 317720 27 497649.51 104.25 100.00 316222- 198319 27 227523.94 69.13 100.00 197139- 155270 27 174079.19 60.19 100.00 155157- 107870 27 133066.75 38.85 100.00 107538- 85319 27 97462.88 32.77 100.00 83752- 6470 27 53072.84 22.95 100.00 6428- 3523 27 4856.64 5.14 92.59 3496- 1120 36 2707.51 4.24 77.78 ------------------------------------------------------------------------------------ 4199082- 1120 279 410463.60 56.95 96.42 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 27 727864.83 99.39 100.00 1.39- 1.12 27 660709.91 60.23 100.00 1.12- 0.98 27 588379.14 83.53 100.00 0.96- 0.88 27 436971.49 69.69 96.30 0.88- 0.81 27 553187.15 75.57 100.00 0.81- 0.75 27 265122.72 43.20 100.00 0.75- 0.71 27 262669.43 42.23 100.00 0.71- 0.67 27 291362.04 42.45 85.19 0.67- 0.64 27 233688.16 35.11 96.30 0.64- 0.58 36 166126.77 27.85 88.89 ------------------------------------------------------------------------------------ 4.82- 0.58 279 410463.60 56.95 96.42 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:12:40 2018 Sorting 279 observations 58 unique observations with > 7.00 F2/sig(F2) 279 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Maximum number of 58 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 279 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 216 observations > 7.00 F2/sig(F2) 216 observations in 1 runs Run # start # end # total # 1 0 48 49 Total number of frames 49 Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 216 removed 19 = 197, unique = 58) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 197 observations in 1 runs Run # start # end # total # 1 0 48 49 Total number of frames 49 Frame #15 of 49 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 58 unique data precomputed (should be 58) 58 unique data with 197 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 197 removed 0 = 197, unique = 58) 58 unique data precomputed (should be 58) 58 unique data with 197 observations RMS deviation of equivalent data = 0.05851 Rint = 0.03706 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.03706, wR= 0.06048 Trying model 1 (ne=2, no=0)... Results: Rint= 0.01875, wR= 0.02740, Acormin=0.876, Acormax=1.178, Acor_av=0.966 F test: Probability=1.000, F= 3.766 Trying model 2 (ne=2, no=1)... Results: Rint= 0.01849, wR= 0.02701, Acormin=0.874, Acormax=1.209, Acor_av=0.971 F test: Probability=0.512, F= 1.006 Trying model 3 (ne=4, no=0)... Results: Rint= 0.01356, wR= 0.01949, Acormin=0.890, Acormax=1.263, Acor_av=0.983 F test: Probability=0.999, F= 1.783 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01335, wR= 0.01909, Acormin=0.882, Acormax=1.272, Acor_av=0.986 F test: Probability=0.517, F= 1.008 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01153, wR= 0.01749, Acormin=0.878, Acormax=1.281, Acor_av=0.989 F test: Probability=0.906, F= 1.274 Final absorption model (ne=4, no=0): Rint= 0.01356, Acormin=0.890, Acormax=1.263, Acor_av=0.983 Combined refinement in use Rint: 0.03722 There are 48 active scales (one needs to be fixed) Refinement control: frame scale #3 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 4, max odd order: 0 (14 parameters) Refinement control: 61 pars with 1891 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.05851 Using Levenberg-Marquardt: 0.00010 New wR= 0.01387 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.03706 with corrections 0.01032 Rint for all data: 0.03722 with corrections 0.01054 0 observations identified as outliers and rejected Cycle 2 wR= 0.01387 Using Levenberg-Marquardt: 0.00001 New wR= 0.01384 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.03706 with corrections 0.01021 Rint for all data: 0.03722 with corrections 0.01044 0 observations identified as outliers and rejected Cycle 3 wR= 0.01384 Using Levenberg-Marquardt: 0.00000 New wR= 0.01388 Using Levenberg-Marquardt: 0.00001 New wR= 0.01388 Using Levenberg-Marquardt: 0.00010 New wR= 0.01388 Using Levenberg-Marquardt: 0.00100 New wR= 0.01387 Using Levenberg-Marquardt: 0.01000 New wR= 0.01385 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.03706 with corrections 0.01024 Rint for all data: 0.03722 with corrections 0.01047 Final wR= 0.01385 Final frame scales: Min= 0.9728 Max= 1.0494 Final absorption correction factors: Amin= 0.7974 Amax= 1.0728 PROFFIT INFO: Inet (after scale3 abspack): min=1078.5563 max=4414009.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=170.5156 max=46291.1445 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:1/50 279 reflections read from tmp file 24 reflections are rejected (1 as outliers, 23 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 29 14 20 12 0 1 1 Initial Chi^2= 0.19577 Cycle 1, Chi^2= 1.13016 Current error model SIG(F2)^2 = 52.91*I_RAW + 11.63*I_BACK+(0.00906*)^2 Cycle 2, Chi^2= 1.02292 Current error model SIG(F2)^2 = 30.49*I_RAW + 31.15*I_BACK+(0.01498*)^2 Cycle 3, Chi^2= 1.00795 Current error model SIG(F2)^2 = 43.36*I_RAW + 19.56*I_BACK+(0.01256*)^2 Cycle 4, Chi^2= 0.99929 Current error model SIG(F2)^2 = 39.02*I_RAW + 23.37*I_BACK+(0.01357*)^2 Cycle 5, Chi^2= 1.00067 Current error model SIG(F2)^2 = 40.86*I_RAW + 21.69*I_BACK+(0.01318*)^2 Cycle 6, Chi^2= 0.99980 Current error model SIG(F2)^2 = 40.16*I_RAW + 22.32*I_BACK+(0.01333*)^2 Cycle 7, Chi^2= 1.00009 Current error model SIG(F2)^2 = 40.44*I_RAW + 22.07*I_BACK+(0.01327*)^2 Cycle 8, Chi^2= 0.99997 Current error model SIG(F2)^2 = 40.33*I_RAW + 22.17*I_BACK+(0.01330*)^2 Cycle 9, Chi^2= 1.00001 Current error model SIG(F2)^2 = 40.37*I_RAW + 22.13*I_BACK+(0.01329*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 40.37*I_RAW + 22.13*I_BACK+(0.01329*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4414010- 1257568 27 2035452.65 70.51 100.00 1229353- 765382 27 1003965.32 62.29 100.00 764451- 317079 27 497529.45 61.25 100.00 310968- 195001 27 227456.25 51.91 100.00 194999- 160068 27 174724.96 46.69 100.00 158592- 110833 27 130429.01 34.92 100.00 107100- 89602 27 99083.92 30.79 100.00 87014- 6615 27 53046.22 22.95 100.00 6513- 3475 27 4892.93 7.04 100.00 3472- 1079 36 2690.77 5.79 91.67 ------------------------------------------------------------------------------------ 4414010- 1079 279 409371.14 38.33 98.92 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 27 727219.00 57.81 100.00 1.39- 1.12 27 663769.20 44.24 100.00 1.12- 0.98 27 597980.59 46.25 100.00 0.96- 0.88 27 427159.33 44.12 100.00 0.88- 0.81 27 549800.69 46.17 100.00 0.81- 0.75 27 262927.90 31.21 100.00 0.75- 0.71 27 254528.18 33.52 100.00 0.71- 0.67 27 295310.06 32.05 92.59 0.67- 0.64 27 226122.57 28.54 100.00 0.64- 0.58 36 169013.17 24.12 97.22 ------------------------------------------------------------------------------------ 4.82- 0.58 279 409371.14 38.33 98.92 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 27 727219.00 57.81 100.00 4.82- 1.12 54 695494.10 51.03 100.00 4.82- 0.98 81 662989.60 49.44 100.00 4.82- 0.88 108 604032.03 48.11 100.00 4.82- 0.81 135 593185.76 47.72 100.00 4.82- 0.75 162 538142.79 44.97 100.00 4.82- 0.71 189 497626.41 43.33 100.00 4.82- 0.67 216 472336.87 41.92 99.07 4.82- 0.64 243 444979.72 40.43 99.18 4.82- 0.58 279 409371.14 38.33 98.92 ------------------------------------------------------------------------------------ 4.82- 0.58 279 409371.14 38.33 98.92 Scale applied to data: s=0.226551 (maximum obs:4414009.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.010; Rsigma 0.017: data 279 -> merged 100 With outlier rejection... Rint 0.010; Rsigma 0.017: data 276 -> merged 100 Rejected total: 3, method kkm 3, method Blessing 0 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585809, 4.830701 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 8 10 2.13 80.00 17 1.61 - 1.21 10 10 2.60 100.00 26 1.17 - 1.01 10 10 3.30 100.00 33 0.99 - 0.89 10 10 2.80 100.00 28 0.88 - 0.81 10 10 3.30 100.00 33 0.81 - 0.74 10 10 2.60 100.00 26 0.73 - 0.71 10 10 3.20 100.00 32 0.70 - 0.66 9 10 2.56 90.00 23 0.66 - 0.64 10 10 2.50 100.00 25 0.63 - 0.60 8 10 2.63 80.00 21 --------------------------------------------------------------- 5.92 - 0.60 95 100 2.78 95.00 264 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:12:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919271 5.914130 5.920691 59.9685 89.9961 59.9738 263 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 126 133 133 131 196 177 183 263 N (int>3sigma) = 0 113 133 120 117 183 161 165 239 Mean intensity = 0.0 86.5 40.8 86.3 93.1 70.9 103.1 101.5 96.1 Mean int/sigma = 0.0 21.5 21.2 22.2 24.7 21.6 23.8 24.4 23.3 Lattice type: P chosen Volume: 146.44 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 Unitcell: 5.914 5.914 5.915 90.10 119.93 119.94 Niggli form: a.a = 34.977 b.b = 34.980 c.c = 34.982 b.c = -0.063 a.c = -17.452 a.b = -17.459 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.035 [ 123] Vol = 585.7 Cell: 8.372 8.372 8.357 90.01 90.00 90.01 Volume: 585.75 Matrix:-1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.090 RHOMBOHEDRAL R-lattice R(int) = 0.065 [ 41] Vol = 439.3 Cell: 5.919 5.914 14.494 90.09 90.01 120.03 Volume: 439.31 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.090 RHOMBOHEDRAL R-lattice R(int) = 0.093 [ 3] Vol = 439.3 Trigonal Cell: 5.919 5.914 14.494 90.09 90.01 120.03 Volume: 439.31 Matrix:-1.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.008 TETRAGONAL I-lattice R(int) = 0.037 [ 72] Vol = 292.9 Cell: 5.921 5.919 8.357 89.99 89.99 90.00 Volume: 292.87 Matrix: 0.0000 0.0000 -1.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.014 TETRAGONAL I-lattice R(int) = 0.037 [ 72] Vol = 292.9 Cell: 5.919 5.921 8.357 90.01 90.01 90.00 Volume: 292.87 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.007 ORTHORHOMBIC I-lattice R(int) = 0.033 [ 120] Vol = 292.9 Cell: 5.919 5.921 8.357 89.99 89.99 90.00 Volume: 292.87 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.046 ORTHORHOMBIC I-lattice R(int) = 0.021 [ 31] Vol = 292.9 Cell: 5.914 8.372 5.915 89.99 89.89 89.99 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.004 MONOCLINIC I-lattice R(int) = 0.029 [ 72] Vol = 292.9 Cell: 5.921 5.919 8.357 90.01 90.01 90.00 Volume: 292.87 Matrix: 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.078 MONOCLINIC I-lattice R(int) = 0.020 [ 27] Vol = 292.9 Cell: 5.914 5.915 8.372 90.01 90.01 89.89 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.008 MONOCLINIC I-lattice R(int) = 0.049 [ 4] Vol = 292.9 Cell: 5.914 8.372 5.915 89.99 90.11 90.01 Volume: 292.87 Matrix: 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 -1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.046 MONOCLINIC I-lattice R(int) = 0.002 [ 1] Vol = 292.9 Cell: 5.915 5.914 8.372 89.99 90.01 90.11 Volume: 292.87 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.080 MONOCLINIC C-lattice R(int) = 0.036 [ 8] Vol = 292.9 Cell: 10.249 5.914 5.915 90.10 125.23 89.94 Volume: 292.87 Matrix:-1.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.000 [ 0] Vol = 146.4 Cell: 5.914 5.914 5.915 90.10 119.93 119.94 Volume: 146.44 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 133 0 179 175 263 N (int>3sigma) = 0 0 0 0 133 0 166 162 239 Mean intensity = 0.0 0.0 0.0 0.0 40.8 0.0 93.0 102.2 96.1 Mean int/sigma = 0.0 0.0 0.0 0.0 21.2 0.0 22.6 24.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.271 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 4 4 22 60 N I>3s 4 4 19 60 1.0 1.0 1.0 47.3 5.8 5.8 4.1 24.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.035 119 Fd-3m 1 1 227 C N N N N 37 2284 0.033 152 0kl, h0l, hhl, with too little data to consider diffraction symbol Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371833 8.372402 8.356829 90.0106 89.9977 90.0137 ZERR 1.00 0.005665 0.001075 0.014481 0.0450 0.0168 0.0123 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4414010- 726096 59 59 25 2.4 1454443.79 65.61 0.008 0.009 670457- 142518 82 82 25 3.3 261595.30 52.16 0.014 0.015 136993- 6837 71 71 25 2.8 94300.42 29.82 0.020 0.022 6577- 1370 67 64 25 2.6 3779.97 6.27 0.092 0.091 ------------------------------------------------------------------------------------------- 4414010- 1370 279 276 100 2.8 413769.01 38.65 0.010 0.011 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 70 69 25 2.8 664528.10 52.25 0.012 0.013 0.015 1.01-0.81 72 71 25 2.8 489274.73 41.76 0.008 0.009 0.016 0.78-0.67 75 74 25 3.0 291034.03 33.62 0.010 0.010 0.020 0.66-0.59 62 62 25 2.5 194722.33 25.94 0.014 0.015 0.023 ------------------------------------------------------------------------------------------------------ inf-0.59 279 276 100 2.8 413769.01 38.65 0.010 0.011 0.017 inf-0.61 265 262 94 2.8 428802.00 39.59 0.010 0.011 0.017 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 69 27 25 92.6 2.8 664528.10 99.14 0.012 0.009 1.01-0.81 71 25 25 100.0 2.8 489274.73 79.91 0.008 0.009 0.78-0.67 74 26 25 96.2 3.0 291034.03 62.24 0.010 0.012 0.66-0.59 62 32 25 78.1 2.5 194722.33 43.28 0.014 0.015 -------------------------------------------------------------------------------------------- inf-0.59 276 110 100 90.9 2.8 413769.01 71.75 0.010 0.010 inf-0.61 262 98 94 95.9 2.8 428802.00 73.90 0.010 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:19:52 2018) ID: 2932; threads 39; handles 878; mem 517664.00 (1237820.00)kB; time: 1w 4d 22h 25m 23s MEMORY INFO: Memory PF:242.0, Ph:420.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.6,peak PF: 697.1, WS: 297.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:244.0, Ph:420.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.4,peak PF: 697.1, WS: 298.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:19:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000023 0.000041 0.000024 ) -0.068858 -0.065594 -0.010716 ( 0.000041 0.000071 0.000043 ) 0.109112 -0.153091 0.115835 ( 0.000041 0.000072 0.000043 ) 5.91502 ( 0.00302 ) 5.91640 ( 0.00317 ) 5.92265 ( 0.00175 ) 60.05206 ( 0.04229 ) 89.98756 ( 0.03143 ) 60.01743 ( 0.05467 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:19:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000023 0.000041 0.000024 ) -0.068858 -0.065594 -0.010716 ( 0.000041 0.000071 0.000043 ) 0.109112 -0.153091 0.115835 ( 0.000041 0.000072 0.000043 ) M - matrix: 0.021561 -0.014406 0.007200 ( 0.000011 0.000012 0.000008 ) -0.014406 0.028816 -0.014405 ( 0.000012 0.000024 0.000012 ) 0.007200 -0.014405 0.021553 ( 0.000008 0.000012 0.000011 ) unit cell: 5.915(3) 5.916(3) 5.9227(17) 60.05(4) 89.99(3) 60.02(5) V = 146.73(10) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb PROFFITPEAK info: 1126 peaks in the peak location table UB fit with 435 obs out of 474 (total:475,skipped:1) (91.77%) UB - matrix: -0.070196 0.030824 0.088676 ( 0.000064 0.000101 0.000055 ) -0.068029 -0.066173 -0.010677 ( 0.000079 0.000124 0.000068 ) 0.109145 -0.153045 0.116304 ( 0.000110 0.000173 0.000094 ) M - matrix: 0.021468 -0.014366 0.007196 ( 0.000028 0.000028 0.000018 ) -0.014366 0.028752 -0.014360 ( 0.000028 0.000056 0.000027 ) 0.007196 -0.014360 0.021504 ( 0.000018 0.000027 0.000024 ) unit cell: 5.934(6) 5.918(6) 5.925(4) 60.04(9) 90.08(7) 59.98(11) V = 147.1(2) UB fit with 435 obs out of 474 (total:475,skipped:1) (91.77%) UB - matrix: -0.070196 0.030824 0.088676 ( 0.000064 0.000101 0.000055 ) -0.068029 -0.066173 -0.010677 ( 0.000079 0.000124 0.000068 ) 0.109145 -0.153045 0.116304 ( 0.000110 0.000173 0.000094 ) M - matrix: 0.021468 -0.014366 0.007196 ( 0.000028 0.000028 0.000018 ) -0.014366 0.028752 -0.014360 ( 0.000028 0.000056 0.000027 ) 0.007196 -0.014360 0.021504 ( 0.000018 0.000027 0.000024 ) unit cell: 5.934(6) 5.918(6) 5.925(4) 60.04(9) 90.08(7) 59.98(11) V = 147.1(2) OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 UB - matrix: -0.070163 0.030713 0.088452 ( 0.000072 0.000112 0.000061 ) -0.068077 -0.065904 -0.010694 ( 0.000074 0.000116 0.000063 ) 0.109039 -0.152868 0.116013 ( 0.000100 0.000156 0.000085 ) M - matrix: 0.021447 -0.014337 0.007172 ( 0.000026 0.000026 0.000017 ) -0.014337 0.028655 -0.014313 ( 0.000026 0.000051 0.000025 ) 0.007172 -0.014313 0.021397 ( 0.000017 0.000025 0.000023 ) UB fit with 439 obs out of 474 (total:475,skipped:1) (92.62%) unit cell: 5.937(6) 5.931(6) 5.942(4) 59.99(9) 90.04(7) 59.97(10) V = 147.83(19) UB fit with 439 obs out of 474 (total:475,skipped:1) (92.62%) UB - matrix: -0.070164 0.030713 0.088452 ( 0.000072 0.000112 0.000061 ) -0.068077 -0.065904 -0.010694 ( 0.000074 0.000116 0.000063 ) 0.109039 -0.152868 0.116013 ( 0.000100 0.000156 0.000085 ) M - matrix: 0.021447 -0.014337 0.007172 ( 0.000026 0.000026 0.000017 ) -0.014337 0.028655 -0.014313 ( 0.000026 0.000051 0.000025 ) 0.007172 -0.014313 0.021397 ( 0.000017 0.000025 0.000023 ) unit cell: 5.937(6) 5.931(6) 5.942(4) 59.99(9) 90.04(7) 59.97(10) V = 147.83(19) OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 475 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Run 1 Omega scan: (-107.000 - -32.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 591 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070164 0.030713 0.088452 ( 0.000072 0.000112 0.000061 ) -0.068077 -0.065904 -0.010694 ( 0.000074 0.000116 0.000063 ) 0.109039 -0.152868 0.116013 ( 0.000100 0.000156 0.000085 ) M - matrix: 0.021447 -0.014337 0.007172 ( 0.000026 0.000026 0.000017 ) -0.014337 0.028655 -0.014313 ( 0.000026 0.000051 0.000025 ) 0.007172 -0.014313 0.021397 ( 0.000017 0.000025 0.000023 ) UB fit with 439 obs out of 474 (total:475,skipped:1) (92.62%) unit cell: 5.937(6) 5.931(6) 5.942(4) 59.99(9) 90.04(7) 59.97(10) V = 147.83(19) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 438 obs out of 474 (total:475,skipped:1) (92.41%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb 4 of 301 peaks identified as outliers and rejected 297 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 297 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 297 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.38 | 30 | 0.970 ( 0.157) | 1.352 ( 0.684) | 1.451 ( 0.963) | 1.33- 1.12 | 30 | 1.056 ( 0.117) | 1.072 ( 0.145) | 1.140 ( 0.454) | 1.12- 0.97 | 30 | 1.064 ( 0.113) | 1.080 ( 0.134) | 1.147 ( 0.499) | 0.96- 0.86 | 30 | 1.087 ( 0.108) | 1.078 ( 0.126) | 1.086 ( 0.429) | 0.86- 0.81 | 30 | 1.134 ( 0.092) | 1.032 ( 0.116) | 1.454 ( 0.518) | 0.78- 0.73 | 30 | 1.114 ( 0.084) | 1.001 ( 0.135) | 1.324 ( 0.500) | 0.73- 0.69 | 30 | 1.122 ( 0.067) | 0.942 ( 0.108) | 1.385 ( 0.487) | 0.69- 0.66 | 30 | 1.112 ( 0.055) | 0.893 ( 0.094) | 1.388 ( 0.526) | 0.66- 0.63 | 30 | 1.087 ( 0.057) | 0.857 ( 0.067) | 1.486 ( 0.539) | 0.63- 0.59 | 27 | 1.055 ( 0.088) | 0.804 ( 0.044) | 1.319 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 297 | 1.080 ( 0.109) | 1.013 ( 0.283) | 1.318 ( 0.581) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 297 obs out of 297 (total:297,skipped:0) (100.00%) UB - matrix: -0.070010 0.030351 0.088678 ( 0.000034 0.000047 0.000024 ) -0.068434 -0.065627 -0.010780 ( 0.000038 0.000052 0.000027 ) 0.109108 -0.152951 0.115752 ( 0.000035 0.000047 0.000025 ) M - matrix: 0.021489 -0.014322 0.007159 ( 0.000010 0.000009 0.000006 ) -0.014322 0.028622 -0.014305 ( 0.000009 0.000016 0.000008 ) 0.007159 -0.014305 0.021378 ( 0.000006 0.000008 0.000007 ) unit cell: 5.927(2) 5.933(2) 5.9463(17) 59.94(4) 90.00(3) 60.01(4) V = 147.76(8) OTKP changes: 297 1 1 1 OTKP changes: 297 1 1 1 OTKP changes: 297 1 1 1 UB - matrix: -0.070088 0.030535 0.088757 ( 0.000031 0.000041 0.000022 ) -0.068240 -0.065927 -0.010766 ( 0.000035 0.000048 0.000025 ) 0.109187 -0.153137 0.116072 ( 0.000032 0.000043 0.000022 ) M - matrix: 0.021491 -0.014362 0.007187 ( 0.000009 0.000008 0.000006 ) -0.014362 0.028730 -0.014355 ( 0.000008 0.000015 0.000007 ) 0.007187 -0.014355 0.021466 ( 0.000006 0.000007 0.000007 ) UB fit with 297 obs out of 297 (total:297,skipped:0) (100.00%) unit cell: 5.929(2) 5.922(2) 5.9327(15) 59.99(3) 90.05(2) 59.99(4) V = 147.20(8) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -32.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 589 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070088 0.030535 0.088757 ( 0.000031 0.000041 0.000022 ) -0.068240 -0.065927 -0.010766 ( 0.000035 0.000048 0.000025 ) 0.109187 -0.153137 0.116072 ( 0.000032 0.000043 0.000022 ) M - matrix: 0.021491 -0.014362 0.007187 ( 0.000009 0.000008 0.000006 ) -0.014362 0.028730 -0.014355 ( 0.000008 0.000015 0.000007 ) 0.007187 -0.014355 0.021466 ( 0.000006 0.000007 0.000007 ) UB fit with 297 obs out of 297 (total:297,skipped:0) (100.00%) unit cell: 5.929(2) 5.922(2) 5.9327(15) 59.99(3) 90.05(2) 59.99(4) V = 147.20(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 297 obs out of 297 (total:297,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb 5 of 297 peaks identified as outliers and rejected 292 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 292 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 292 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.37 | 29 | 0.979 ( 0.160) | 1.263 ( 0.628) | 1.304 ( 0.786) | 1.37- 1.12 | 29 | 1.055 ( 0.112) | 1.146 ( 0.356) | 1.173 ( 0.480) | 1.12- 0.97 | 29 | 1.066 ( 0.109) | 1.090 ( 0.134) | 1.121 ( 0.445) | 0.96- 0.88 | 29 | 1.076 ( 0.105) | 1.074 ( 0.136) | 1.057 ( 0.409) | 0.86- 0.81 | 29 | 1.148 ( 0.079) | 1.057 ( 0.120) | 1.461 ( 0.507) | 0.81- 0.74 | 29 | 1.106 ( 0.090) | 0.987 ( 0.135) | 1.341 ( 0.529) | 0.73- 0.70 | 29 | 1.125 ( 0.069) | 0.967 ( 0.106) | 1.395 ( 0.466) | 0.70- 0.67 | 29 | 1.110 ( 0.057) | 0.886 ( 0.064) | 1.354 ( 0.530) | 0.67- 0.63 | 29 | 1.099 ( 0.047) | 0.877 ( 0.071) | 1.468 ( 0.588) | 0.63- 0.59 | 31 | 1.056 ( 0.076) | 0.804 ( 0.036) | 1.344 ( 0.500) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 292 | 1.082 ( 0.105) | 1.014 ( 0.280) | 1.302 ( 0.549) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-14.2 | 29 | 1.131 ( 0.053) | 1.189 ( 0.185) | 1.203 ( 0.536) | 14.2-19.6 | 29 | 1.135 ( 0.072) | 1.176 ( 0.280) | 1.380 ( 0.641) | 19.6-23.5 | 29 | 1.134 ( 0.090) | 1.166 ( 0.430) | 1.330 ( 0.534) | 23.6-27.7 | 29 | 1.127 ( 0.097) | 1.210 ( 0.442) | 1.459 ( 0.554) | 27.7-30.9 | 29 | 1.066 ( 0.101) | 1.005 ( 0.107) | 1.292 ( 0.483) | 31.0-33.7 | 29 | 1.087 ( 0.087) | 0.942 ( 0.104) | 1.244 ( 0.522) | 34.0-36.9 | 29 | 1.064 ( 0.083) | 0.888 ( 0.076) | 1.446 ( 0.559) | 37.0-39.3 | 29 | 1.038 ( 0.107) | 0.913 ( 0.178) | 1.267 ( 0.487) | 39.3-42.3 | 29 | 0.993 ( 0.120) | 0.833 ( 0.102) | 1.192 ( 0.546) | 42.4-49.3 | 31 | 1.046 ( 0.114) | 0.829 ( 0.069) | 1.217 ( 0.536) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.3 | 292 | 1.082 ( 0.105) | 1.014 ( 0.280) | 1.302 ( 0.549) | Fitted profile normalization line parameters e1 dimension: a=-0.0021 b=1.10 e2 dimension: a=-0.0103 b=1.27 e3 dimension: a=0.0054 b=0.93 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 4105 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706834 Maximum peak integral for reflections I/sig<= 10000 - raw: 8009297 lp-corr: 2102700 PROFFITPEAK - Finished at Tue Mar 27 13:19:58 2018 PROFFITMAIN - Started at Tue Mar 27 13:19:58 2018 OTKP changes: 292 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 292 1 1 1 OTKP changes: 292 1 1 1 OTKP changes: 292 1 1 1 UB - matrix: -0.070076 0.030511 0.088783 ( 0.000030 0.000041 0.000022 ) -0.068257 -0.065887 -0.010776 ( 0.000032 0.000043 0.000023 ) 0.109155 -0.153113 0.116036 ( 0.000030 0.000041 0.000022 ) M - matrix: 0.021485 -0.014354 0.007180 ( 0.000009 0.000008 0.000005 ) -0.014354 0.028716 -0.014348 ( 0.000008 0.000014 0.000007 ) 0.007180 -0.014348 0.021463 ( 0.000005 0.000007 0.000006 ) UB fit with 292 obs out of 292 (total:292,skipped:0) (100.00%) unit cell: 5.929(2) 5.923(2) 5.9327(15) 59.99(3) 90.03(2) 59.99(4) V = 147.24(7) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -32.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 591 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070076 0.030511 0.088783 ( 0.000030 0.000041 0.000022 ) -0.068257 -0.065887 -0.010776 ( 0.000032 0.000043 0.000023 ) 0.109155 -0.153113 0.116036 ( 0.000030 0.000041 0.000022 ) M - matrix: 0.021485 -0.014354 0.007180 ( 0.000009 0.000008 0.000005 ) -0.014354 0.028716 -0.014348 ( 0.000008 0.000014 0.000007 ) 0.007180 -0.014348 0.021463 ( 0.000005 0.000007 0.000006 ) UB fit with 292 obs out of 292 (total:292,skipped:0) (100.00%) unit cell: 5.929(2) 5.923(2) 5.9327(15) 59.99(3) 90.03(2) 59.99(4) V = 147.24(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 292 obs out of 292 (total:292,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070076 0.030511 0.088783 ( 0.000030 0.000041 0.000022 ) -0.068257 -0.065887 -0.010776 ( 0.000032 0.000043 0.000023 ) 0.109155 -0.153113 0.116036 ( 0.000030 0.000041 0.000022 ) M - matrix: 0.021485 -0.014354 0.007180 ( 0.000009 0.000008 0.000005 ) -0.014354 0.028716 -0.014348 ( 0.000008 0.000014 0.000007 ) 0.007180 -0.014348 0.021463 ( 0.000005 0.000007 0.000006 ) UB fit with 292 obs out of 292 (total:292,skipped:0) (100.00%) unit cell: 5.929(2) 5.923(2) 5.9327(15) 59.99(3) 90.03(2) 59.99(4) V = 147.24(7) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070076 0.030511 0.088783 ( 0.000030 0.000041 0.000022 ) -0.068257 -0.065887 -0.010776 ( 0.000032 0.000043 0.000023 ) 0.109155 -0.153113 0.116036 ( 0.000030 0.000041 0.000022 ) M - matrix: 0.021485 -0.014354 0.007180 ( 0.000009 0.000008 0.000005 ) -0.014354 0.028716 -0.014348 ( 0.000008 0.000014 0.000007 ) 0.007180 -0.014348 0.021463 ( 0.000005 0.000007 0.000006 ) UB fit with 292 obs out of 292 (total:292,skipped:0) (100.00%) unit cell: 5.929(2) 5.923(2) 5.9327(15) 59.99(3) 90.03(2) 59.99(4) V = 147.24(7) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 17 reflections under beam stop or inside a detector rejection region 1 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof 428 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:19:59 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -32.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=222.0000 max=12239915.0000 PROFFIT INFO: signal sum lp corr: min=703.3810 max=2956833.1674 PROFFIT INFO: background sum: min=1300.0000 max=7176.0000 PROFFIT INFO: background sum sig2: min=682.0000 max=6802.0000 PROFFIT INFO: num of signal pixels: min=64 max=558 PROFFIT INFO: Inet: min=1125.4095 max=4730933.5000 PROFFIT INFO: sig(Inet): min=183.2870 max=46958.9805 PROFFIT INFO: Inet/sig(Inet): min=1.06 max=228.11 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 3 14 42 97 107 169 278 383 428 Percent 0.0 0.0 0.7 3.3 9.8 22.7 25.0 39.5 65.0 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 428 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 428 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4730934- 1355782 42 2097614.69 130.05 100.00 1322395- 799956 42 1020275.90 112.48 100.00 798140- 315947 42 486916.79 102.12 100.00 311726- 189225 42 221463.22 68.00 100.00 186282- 154588 42 170968.90 57.85 100.00 152491- 102730 42 125684.24 37.47 100.00 102277- 81145 42 91268.29 30.67 100.00 77975- 5792 42 39949.37 18.92 100.00 5634- 3497 42 4402.72 6.01 95.24 3454- 1125 50 2693.47 4.17 76.00 ------------------------------------------------------------------------------------ 4730934- 1125 428 418209.17 55.79 96.73 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.18 42 749507.20 88.17 100.00 1.18- 0.96 42 621718.15 59.73 100.00 0.96- 0.85 42 630090.48 74.04 100.00 0.83- 0.75 42 465842.14 72.72 100.00 0.75- 0.72 42 363272.61 55.95 97.62 0.72- 0.65 42 396776.41 58.11 97.62 0.65- 0.61 42 195713.93 34.00 90.48 0.61- 0.57 42 356702.40 48.73 92.86 0.57- 0.53 42 245684.13 39.68 100.00 0.53- 0.42 50 198612.28 31.41 90.00 ------------------------------------------------------------------------------------ 5.27- 0.42 428 418209.17 55.79 96.73 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:19:59 2018 Sorting 428 observations 104 unique observations with > 7.00 F2/sig(F2) 428 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Maximum number of 104 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 428 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 333 observations > 7.00 F2/sig(F2) 333 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Frame #58 of 75 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 2.4 (Out of 333 removed 108 = 225, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 225 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Frame #14 of 75 skipped from refinement Frame #15 of 75 skipped from refinement Frame #23 of 75 skipped from refinement Frame #30 of 75 skipped from refinement Frame #58 of 75 skipped from refinement Frame #64 of 75 skipped from refinement 6 frames need to be skipped from refinement, because of missing redundant and/or observable data 93 unique data precomputed (should be 93) 93 unique data with 225 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 2.4 (Out of 225 removed 0 = 225, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 225 observations RMS deviation of equivalent data = 0.56456 Rint = 0.42705 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.40015, wR= 5.28003 Trying model 1 (ne=2, no=0)... Results: Rint= 0.55462, wR= 1.98340, Acormin=-0.400, Acormax=0.839, Acor_av=0.208 F test: Probability=0.000, F= 0.501 Trying model 2 (ne=2, no=1)... Results: Rint= 0.76483, wR= 3.78264, Acormin=-0.278, Acormax=0.639, Acor_av=0.025 F test: Probability=0.000, F= 0.257 Trying model 3 (ne=4, no=0)... Results: Rint= 0.35143, wR= 1.13927, Acormin=-0.099, Acormax=1.118, Acor_av=0.150 F test: Probability=0.791, F= 1.158 Trying model 4 (ne=4, no=1)... Results: Rint= 0.48278, wR= 2.88418, Acormin=-0.076, Acormax=0.421, Acor_av=0.078 F test: Probability=0.000, F= 0.598 Trying model 5 (ne=4, no=3)... Results: Rint= 0.49422, wR= 2.19352, Acormin=-0.067, Acormax=0.173, Acor_av=0.015 F test: Probability=0.000, F= 0.535 Trying model 6 (ne=6, no=0)... Results: Rint= 0.40632, wR= 1.35465, Acormin=-0.057, Acormax=0.390, Acor_av=0.038 F test: Probability=0.000, F= 0.770 Trying model 7 (ne=6, no=1)... Results: Rint= 0.29918, wR= 1.88934, Acormin=-0.067, Acormax=0.266, Acor_av=0.037 F test: Probability=0.954, F= 1.379 Trying model 8 (ne=6, no=3)... Results: Rint= 0.30191, wR= 0.65307, Acormin=-0.042, Acormax=0.214, Acor_av=0.024 F test: Probability=0.883, F= 1.260 Trying model 9 (ne=6, no=5)... Results: Rint= 0.16750, wR= 0.97393, Acormin=-0.036, Acormax=0.159, Acor_av=0.022 F test: Probability=1.000, F= 3.616 Trying model 10 (ne=8, no=0)... Results: Rint= 0.20481, wR= 1.36536, Acormin=-0.015, Acormax=0.219, Acor_av=0.029 F test: Probability=1.000, F= 2.535 Trying model 11 (ne=8, no=1)... Results: Rint= 0.18915, wR= 1.46572, Acormin=-0.016, Acormax=0.193, Acor_av=0.028 F test: Probability=1.000, F= 2.870 Trying model 12 (ne=8, no=3)... Results: Rint= 0.11959, wR= 0.42709, Acormin=-0.046, Acormax=0.274, Acor_av=0.038 F test: Probability=1.000, F= 6.580 Trying model 13 (ne=8, no=5)... Results: Rint= 0.10389, wR= 0.54136, Acormin=-0.096, Acormax=0.480, Acor_av=0.056 F test: Probability=1.000, F= 7.474 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08598, wR= 0.25103, Acormin=-0.190, Acormax=0.911, Acor_av=0.099 F test: Probability=1.000, F= 8.432 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.61177 There are 69 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 73 pars with 2701 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.56456 Using Levenberg-Marquardt: 0.00010 New wR= 0.57588 Using Levenberg-Marquardt: 0.00100 New wR= 0.51338 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.53494 Rint for all data: 0.61177 with corrections 0.73326 0 observations identified as outliers and rejected Cycle 2 wR= 0.51338 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.53865 Using Levenberg-Marquardt: 10.00000 New wR= 0.50406 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.57339 Rint for all data: 0.61177 with corrections 0.77373 0 observations identified as outliers and rejected Cycle 3 wR= 0.50406 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.49454 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.95817 Rint for all data: 0.61177 with corrections 1.23107 0 observations identified as outliers and rejected Cycle 4 wR= 0.49454 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1000.00000 New wR= 0.49429 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.97804 Rint for all data: 0.61177 with corrections 1.25800 Final wR= 0.49429 Frame scales out of range! Final absorption correction factors: Amin= 0.8073 Amax= 2.7207 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 69 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 73 pars with 2701 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.87699 Using Levenberg-Marquardt: 0.00010 New wR= 0.52630 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.37496 Rint for all data: 0.61177 with corrections 0.60030 0 observations identified as outliers and rejected Cycle 2 wR= 0.52630 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.50172 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.37979 Rint for all data: 0.61177 with corrections 0.61168 0 observations identified as outliers and rejected Cycle 3 wR= 0.50172 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.48160 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.41815 Rint for all data: 0.61177 with corrections 0.63993 0 observations identified as outliers and rejected Cycle 4 wR= 0.48160 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.48095 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.57122 Rint for all data: 0.61177 with corrections 0.73038 0 observations identified as outliers and rejected Cycle 5 wR= 0.48095 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.46707 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.42705 with corrections 0.48251 Rint for all data: 0.61177 with corrections 0.67806 0 observations identified as outliers and rejected Final wR= 0.46707 Final frame scales: Min= 1.0000 Max= 9.4176 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 65 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 64 pars with 2080 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.78699 Using Levenberg-Marquardt: 0.00010 New wR= 0.58039 There are 7 clusters with unrefined scales (size 1-4) Rint for refined data: 0.42705 with corrections 0.44760 Rint for all data: 0.61177 with corrections 0.62631 0 observations identified as outliers and rejected Cycle 2 wR= 0.54626 Using Levenberg-Marquardt: 0.00001 New wR= 0.69157 Using Levenberg-Marquardt: 0.00010 New wR= 0.68910 Using Levenberg-Marquardt: 0.00100 New wR= 0.66321 Using Levenberg-Marquardt: 0.01000 New wR= 0.49455 There are 7 clusters with unrefined scales (size 1-4) Rint for refined data: 0.42705 with corrections 0.52236 Rint for all data: 0.61177 with corrections 0.72451 0 observations identified as outliers and rejected Cycle 3 wR= 0.54299 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.52975 There are 7 clusters with unrefined scales (size 1-4) Rint for refined data: 0.42705 with corrections 0.47976 Rint for all data: 0.61177 with corrections 0.66997 0 observations identified as outliers and rejected Cycle 4 wR= 0.51766 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.51723 There are 7 clusters with unrefined scales (size 1-4) Rint for refined data: 0.42705 with corrections 0.46518 Rint for all data: 0.61177 with corrections 0.65864 Final wR= 0.51723 Final frame scales: Min= 0.2657 Max= 4.4662 1 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=587.1822 max=6331321.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=84.8807 max=80815.6016 PROFFIT INFO: 3 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:1/75 425 reflections read from tmp file 381 reflections are rejected (251 as outliers, 130 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 20 0 1 Initial Chi^2= 1.14091 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.52507 Current error model SIG(F2)^2 = 42.86*I_RAW + 278.56*I_BACK+(0.06388*)^2 Cycle 2, Chi^2= 1.00097 Current error model SIG(F2)^2 = 42.86*I_RAW + 132.26*I_BACK+(0.04151*)^2 Cycle 3, Chi^2= 1.03651 Current error model SIG(F2)^2 = 42.86*I_RAW + 138.76*I_BACK+(0.03802*)^2 Cycle 4, Chi^2= 1.05300 Current error model SIG(F2)^2 = 42.86*I_RAW + 140.00*I_BACK+(0.03686*)^2 Cycle 5, Chi^2= 1.05906 Current error model SIG(F2)^2 = 42.86*I_RAW + 140.57*I_BACK+(0.03643*)^2 Cycle 6, Chi^2= 1.06145 Current error model SIG(F2)^2 = 42.86*I_RAW + 140.80*I_BACK+(0.03626*)^2 Cycle 7, Chi^2= 1.06240 Current error model SIG(F2)^2 = 42.86*I_RAW + 140.90*I_BACK+(0.03619*)^2 Final Chi^2= 1.06240 Final error model SIG(F2)^2 = 42.86*I_RAW + 140.90*I_BACK+(0.03619*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6331322- 1170032 42 2464933.14 94.07 100.00 1159483- 621069 42 867328.31 81.86 100.00 611951- 292730 42 433250.47 52.79 100.00 290379- 187931 42 236279.31 36.31 100.00 187231- 127876 42 153860.67 34.06 100.00 125346- 84424 42 99889.04 23.99 100.00 84263- 52841 42 68720.01 22.86 100.00 52559- 5394 42 25176.82 11.75 83.33 5390- 2816 42 4097.58 4.31 64.29 2795- 587 47 1898.13 3.76 57.45 ------------------------------------------------------------------------------------ 6331322- 587 425 430441.64 36.19 90.12 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.18 42 791864.39 62.92 100.00 1.18- 0.96 42 527270.22 61.71 100.00 0.96- 0.85 42 655931.14 47.32 90.48 0.83- 0.75 42 390628.61 32.42 92.86 0.75- 0.72 42 296183.76 39.52 90.48 0.72- 0.65 42 571425.60 27.98 95.24 0.65- 0.61 42 163619.29 23.14 80.95 0.61- 0.57 42 402242.12 24.48 83.33 0.57- 0.53 42 284452.39 24.69 85.71 0.53- 0.42 47 243101.30 19.69 82.98 ------------------------------------------------------------------------------------ 5.27- 0.42 425 430441.64 36.19 90.12 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.18 42 791864.39 62.92 100.00 5.27- 0.96 84 659567.30 62.32 100.00 5.27- 0.85 126 658355.25 57.32 96.83 5.27- 0.75 168 591423.59 51.09 95.83 5.27- 0.72 210 532375.63 48.78 94.76 5.27- 0.65 252 538883.96 45.31 94.84 5.27- 0.61 294 485274.72 42.15 92.86 5.27- 0.57 336 474895.64 39.94 91.67 5.27- 0.53 378 453735.28 38.24 91.01 5.27- 0.42 425 430441.64 36.19 90.12 ------------------------------------------------------------------------------------ 5.27- 0.42 425 430441.64 36.19 90.12 Scale applied to data: s=0.157945 (maximum obs:6331321.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.617; Rsigma 0.026: data 425 -> merged 232 With outlier rejection... Rint 0.439; Rsigma 0.029: data 378 -> merged 232 Rejected total: 47, method kkm 47, method Blessing 0 Completeness direct cell (a, b, c) = (5.281, 5.281, 5.281), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.425520, 5.280559 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.46 13 15 1.54 86.67 20 1.46 - 1.13 12 15 2.08 80.00 25 1.08 - 0.96 14 15 1.79 93.33 25 0.96 - 0.86 15 15 2.00 100.00 30 0.86 - 0.79 15 15 1.87 100.00 28 0.79 - 0.73 15 15 1.93 100.00 29 0.73 - 0.69 14 15 1.79 93.33 25 0.69 - 0.65 15 15 1.73 100.00 26 0.65 - 0.64 15 15 1.60 100.00 24 0.63 - 0.60 20 21 1.60 95.24 32 --------------------------------------------------------------- 5.93 - 0.60 148 156 1.78 94.87 264 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:20:00 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929479 5.923028 5.932701 59.9878 90.0320 59.9914 378 Reflections read from file xs1714a.hkl; mean (I/sigma) = 31.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 187 181 192 190 280 254 254 378 N (int>3sigma) = 0 167 181 172 168 260 226 225 338 Mean intensity = 0.0 60.6 24.4 59.6 55.8 48.6 71.7 61.3 64.2 Mean int/sigma = 0.0 31.0 29.9 31.8 31.2 30.9 31.4 29.8 31.5 Lattice type: P chosen Volume: 147.24 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.923 5.925 5.926 119.92 90.10 119.94 Niggli form: a.a = 35.082 b.b = 35.111 c.c = 35.117 b.c = -17.515 a.c = -0.059 a.b = -17.517 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.075 CUBIC F-lattice R(int) = 0.330 [ 230] Vol = 589.0 Cell: 8.371 8.390 8.385 90.03 89.97 90.01 Volume: 588.98 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.075 RHOMBOHEDRAL R-lattice R(int) = 0.340 [ 119] Vol = 441.7 Cell: 5.925 5.923 14.525 89.91 90.11 119.94 Volume: 441.73 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.075 RHOMBOHEDRAL R-lattice R(int) = 0.374 [ 24] Vol = 441.7 Trigonal Cell: 5.925 5.923 14.525 89.91 90.11 119.94 Volume: 441.73 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.051 TETRAGONAL I-lattice R(int) = 0.350 [ 150] Vol = 294.5 Cell: 5.929 5.933 8.371 89.97 89.99 90.03 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.055 TETRAGONAL I-lattice R(int) = 0.350 [ 150] Vol = 294.5 Cell: 5.929 5.933 8.371 89.97 89.99 90.03 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.048 ORTHORHOMBIC I-lattice R(int) = 0.358 [ 197] Vol = 294.5 Cell: 5.929 8.371 5.933 89.97 89.97 90.01 Volume: 294.49 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.030 MONOCLINIC I-lattice R(int) = 0.308 [ 107] Vol = 294.5 Cell: 8.371 5.929 5.933 90.03 90.03 90.01 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.063 MONOCLINIC I-lattice R(int) = 0.260 [ 41] Vol = 294.5 Cell: 5.926 5.923 8.390 90.01 90.03 89.90 Volume: 294.49 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.022 MONOCLINIC C-lattice R(int) = 0.257 [ 31] Vol = 294.5 Cell: 8.371 8.390 5.923 90.01 134.94 90.01 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.423 [ 3] Vol = 147.2 Cell: 5.923 5.925 5.926 119.92 90.10 119.94 Volume: 147.24 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 181 0 254 256 378 N (int>3sigma) = 0 0 0 0 181 0 226 232 338 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 71.7 65.0 64.2 Mean int/sigma = 0.0 0.0 0.0 0.0 29.9 0.0 31.4 32.5 31.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.334 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 6 6 36 79 N I>3s 6 6 27 79 0.6 0.6 0.6 27.0 10.7 10.7 5.4 32.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.330 213 Fd-3m 1 1 227 C N N N N 37 2284 0.394 249 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371451 8.390170 8.385486 90.0311 89.9720 90.0125 ZERR 1.00 0.009950 0.004283 0.000723 0.0059 0.0320 0.0074 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 6331322- 1035702 43 38 25 1.5 1980479.85 38.25 0.278 0.278 1008202- 542110 46 44 25 1.8 790995.74 57.01 0.562 0.552 540945- 326052 62 50 25 2.0 358855.11 48.84 0.703 0.691 324866- 215622 46 42 25 1.7 249540.54 34.90 0.525 0.555 210351- 128752 56 45 25 1.8 146341.53 30.02 0.304 0.286 126180- 87576 50 42 25 1.7 103595.70 26.81 0.260 0.260 86522- 60788 37 36 25 1.4 71566.60 21.57 0.329 0.329 60111- 8252 41 37 25 1.5 39359.10 16.32 0.331 0.331 6977- 1216 44 44 32 1.4 3370.72 3.75 0.307 0.320 ------------------------------------------------------------------------------------------- 6331322- 1216 425 378 232 1.6 406356.85 31.46 0.439 0.431 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.13 54 45 25 1.8 715573.37 55.68 0.526 0.506 0.027 1.08-0.88 61 48 25 1.9 498999.63 39.59 0.355 0.359 0.019 0.87-0.75 59 47 26 1.8 358136.67 28.75 0.383 0.383 0.032 0.75-0.69 54 47 25 1.9 533876.29 35.71 0.266 0.243 0.029 0.68-0.64 45 41 25 1.6 320289.96 26.62 0.508 0.508 0.028 0.64-0.59 43 42 26 1.6 374944.23 24.59 0.488 0.488 0.032 0.59-0.56 38 37 25 1.5 147342.06 21.67 0.681 0.681 0.035 0.56-0.53 33 33 25 1.3 401050.49 23.67 0.656 0.656 0.034 0.52-0.43 38 38 30 1.3 209463.90 19.73 0.929 0.929 0.035 ------------------------------------------------------------------------------------------------------ inf-0.43 425 378 232 1.6 406356.85 31.46 0.439 0.431 0.029 inf-0.60 310 264 148 1.8 468390.69 35.62 0.407 0.398 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.13 45 30 25 83.3 1.8 715573.37 96.14 0.526 0.015 1.08-0.88 48 26 25 96.2 1.9 498999.63 63.55 0.355 0.012 0.87-0.75 47 26 26 100.0 1.8 358136.67 42.59 0.383 0.021 0.75-0.69 47 26 25 96.2 1.9 533876.29 60.30 0.266 0.020 0.68-0.64 41 25 25 100.0 1.6 320289.96 39.51 0.508 0.019 0.64-0.59 42 27 26 96.3 1.6 374944.23 36.47 0.488 0.021 0.59-0.56 37 31 25 80.6 1.5 147342.06 32.37 0.681 0.022 0.56-0.53 33 35 25 71.4 1.3 401050.49 31.90 0.656 0.018 0.52-0.43 38 180 30 16.7 1.3 209463.90 27.30 0.929 0.017 -------------------------------------------------------------------------------------------- inf-0.43 378 407 232 57.0 1.6 406356.85 49.35 0.439 0.018 inf-0.60 264 156 148 94.9 1.8 468390.69 57.44 0.407 0.017 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.015256 -0.079430 0.024609 ( 0.000021 0.000012 0.000015 ) 0.032944 -0.028741 -0.072460 ( 0.000022 0.000013 0.000015 ) 0.076556 -0.003440 0.036039 ( 0.000021 0.000012 0.000014 ) M - matrix: 0.007179 0.000002 -0.000004 ( 0.000004 0.000002 0.000002 ) 0.000002 0.007147 0.000004 ( 0.000002 0.000002 0.000002 ) -0.000004 0.000004 0.007155 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.015256 -0.079430 0.024609 ( 0.000021 0.000012 0.000015 ) 0.032944 -0.028741 -0.072460 ( 0.000022 0.000013 0.000015 ) 0.076556 -0.003440 0.036039 ( 0.000021 0.000012 0.000014 ) M - matrix: 0.007151 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007151 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007151 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3715(19) 8.3902(13) 8.3855(16) 90.031(14) 89.972(17) 90.012(16) V = 589.0(2) unit cell: 8.3824(5) 8.3824(5) 8.3824(5) 90.0 90.0 90.0 V = 588.98(6) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -32.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=222.0000 max=12239915.0000 PROFFIT INFO: signal sum lp corr: min=703.3810 max=2956833.1674 PROFFIT INFO: background sum: min=1300.0000 max=7176.0000 PROFFIT INFO: background sum sig2: min=682.0000 max=6802.0000 PROFFIT INFO: num of signal pixels: min=64 max=558 PROFFIT INFO: Inet: min=1125.4095 max=4730933.5000 PROFFIT INFO: sig(Inet): min=183.2870 max=46958.9805 PROFFIT INFO: Inet/sig(Inet): min=1.06 max=228.11 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 6 28 84 194 214 338 556 766 856 Percent 0.0 0.0 0.7 3.3 9.8 22.7 25.0 39.5 65.0 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 428 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 428 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4730934- 1355782 42 2097614.69 130.05 100.00 1322395- 799956 42 1020275.90 112.48 100.00 798140- 315947 42 486916.79 102.12 100.00 311726- 189225 42 221463.22 68.00 100.00 186282- 154588 42 170968.90 57.85 100.00 152491- 102730 42 125684.24 37.47 100.00 102277- 81145 42 91268.29 30.67 100.00 77975- 5792 42 39949.37 18.92 100.00 5634- 3497 42 4402.72 6.01 95.24 3454- 1125 50 2693.47 4.17 76.00 ------------------------------------------------------------------------------------ 4730934- 1125 428 418209.17 55.79 96.73 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 42 769107.78 94.37 100.00 1.39- 1.12 42 790191.49 63.25 100.00 1.12- 0.97 42 536091.60 76.80 100.00 0.97- 0.88 42 387611.89 63.38 97.62 0.88- 0.81 42 552910.67 77.11 100.00 0.81- 0.75 42 257737.45 40.88 100.00 0.75- 0.71 42 234311.75 39.42 95.24 0.71- 0.67 42 317348.86 46.18 90.48 0.66- 0.63 42 208026.35 31.80 90.48 0.63- 0.59 50 175066.75 29.65 94.00 ------------------------------------------------------------------------------------ 4.83- 0.59 428 418209.17 55.79 96.73 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:20:00 2018 Sorting 428 observations 70 unique observations with > 7.00 F2/sig(F2) 428 observations in 1 runs Run # start # end # total # 1 0 74 75 Total number of frames 75 Maximum number of 70 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 428 observations in 1 runs Run # start # end # total # 1 0 37 38 Total number of frames 38 333 observations > 7.00 F2/sig(F2) 333 observations in 1 runs Run # start # end # total # 1 0 37 38 Total number of frames 38 Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 333 removed 13 = 320, unique = 70) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 320 observations in 1 runs Run # start # end # total # 1 0 37 38 Total number of frames 38 70 unique data precomputed (should be 70) 70 unique data with 320 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.6 (Out of 320 removed 0 = 320, unique = 70) 70 unique data precomputed (should be 70) 70 unique data with 320 observations RMS deviation of equivalent data = 0.06112 Rint = 0.05267 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.05267, wR= 0.06663 Trying model 1 (ne=2, no=0)... Results: Rint= 0.03001, wR= 0.03693, Acormin=0.823, Acormax=1.133, Acor_av=0.912 F test: Probability=1.000, F= 3.018 Trying model 2 (ne=2, no=1)... Results: Rint= 0.02856, wR= 0.03363, Acormin=0.852, Acormax=1.221, Acor_av=0.928 F test: Probability=0.751, F= 1.091 Trying model 3 (ne=4, no=0)... Results: Rint= 0.01951, wR= 0.02496, Acormin=0.857, Acormax=1.299, Acor_av=0.974 F test: Probability=1.000, F= 2.281 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01862, wR= 0.02320, Acormin=0.871, Acormax=1.270, Acor_av=0.980 F test: Probability=0.731, F= 1.084 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01726, wR= 0.02152, Acormin=0.880, Acormax=1.323, Acor_av=0.984 F test: Probability=0.936, F= 1.223 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01534, wR= 0.01931, Acormin=0.874, Acormax=1.295, Acor_av=0.985 F test: Probability=0.999, F= 1.528 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01471, wR= 0.01870, Acormin=0.872, Acormax=1.306, Acor_av=0.986 F test: Probability=0.697, F= 1.072 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01456, wR= 0.01778, Acormin=0.869, Acormax=1.305, Acor_av=0.987 F test: Probability=0.663, F= 1.059 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01423, wR= 0.01677, Acormin=0.870, Acormax=1.304, Acor_av=0.988 F test: Probability=0.643, F= 1.052 Final absorption model (ne=6, no=0): Rint= 0.01534, Acormin=0.874, Acormax=1.295, Acor_av=0.985 Combined refinement in use Rint: 0.05282 There are 38 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 0 (27 parameters) Refinement control: 64 pars with 2080 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.06112 Using Levenberg-Marquardt: 0.00010 New wR= 0.01561 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.05267 with corrections 0.01295 Rint for all data: 0.05282 with corrections 0.01319 0 observations identified as outliers and rejected Cycle 2 wR= 0.01561 Using Levenberg-Marquardt: 0.00001 New wR= 0.01549 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.05267 with corrections 0.01291 Rint for all data: 0.05282 with corrections 0.01315 0 observations identified as outliers and rejected Cycle 3 wR= 0.01549 Using Levenberg-Marquardt: 0.00000 New wR= 0.01552 Using Levenberg-Marquardt: 0.00001 New wR= 0.01552 Using Levenberg-Marquardt: 0.00010 New wR= 0.01552 Using Levenberg-Marquardt: 0.00100 New wR= 0.01552 Using Levenberg-Marquardt: 0.01000 New wR= 0.01552 Using Levenberg-Marquardt: 0.10000 New wR= 0.01551 Using Levenberg-Marquardt: 1.00000 New wR= 0.01550 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.05267 with corrections 0.01293 Rint for all data: 0.05282 with corrections 0.01317 Final wR= 0.01550 Final frame scales: Min= 0.9534 Max= 1.0155 Final absorption correction factors: Amin= 0.7404 Amax= 1.1063 PROFFIT INFO: Inet (after scale3 abspack): min=1042.5803 max=4612682.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=180.0998 max=44856.5352 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:1/75 428 reflections read from tmp file 18 reflections are rejected (4 as outliers, 14 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 16 17 19 9 12 10 3 1 3 Initial Chi^2= 0.25814 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.62472 Current error model SIG(F2)^2 = 89.27*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 234.30*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 234.30*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4612682- 1380579 42 2122987.65 103.92 100.00 1350150- 760905 42 1005829.64 47.97 100.00 756287- 313718 42 485729.13 49.57 100.00 313377- 192596 42 223244.63 30.76 100.00 192532- 155006 42 172127.58 24.11 100.00 154383- 104846 42 120892.80 16.23 100.00 103798- 83514 42 93721.93 13.48 100.00 82411- 5644 42 39269.58 9.14 100.00 5596- 3402 42 4391.64 3.70 66.67 3400- 1043 50 2693.12 3.01 38.00 ------------------------------------------------------------------------------------ 4612682- 1043 428 419156.14 29.68 89.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 42 774973.38 68.33 100.00 1.39- 1.12 42 805924.49 50.71 92.86 1.12- 0.97 42 551672.08 36.45 92.86 0.97- 0.88 42 381623.88 27.61 88.10 0.88- 0.81 42 547201.45 33.32 100.00 0.81- 0.75 42 258241.77 18.18 88.10 0.75- 0.71 42 224805.36 17.46 88.10 0.71- 0.67 42 314059.91 20.21 85.71 0.66- 0.63 42 203429.73 14.30 78.57 0.63- 0.59 50 175953.63 13.34 82.00 ------------------------------------------------------------------------------------ 4.83- 0.59 428 419156.14 29.68 89.49 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 42 774973.38 68.33 100.00 4.83- 1.12 84 790448.93 59.52 96.43 4.83- 0.97 126 710856.65 51.83 95.24 4.83- 0.88 168 628548.46 45.77 93.45 4.83- 0.81 210 612279.05 43.28 94.76 4.83- 0.75 252 553272.84 39.10 93.65 4.83- 0.71 294 506348.92 36.01 92.86 4.83- 0.67 336 482312.79 34.03 91.96 4.83- 0.63 378 451325.78 31.84 90.48 4.83- 0.59 428 419156.14 29.68 89.49 ------------------------------------------------------------------------------------ 4.83- 0.59 428 419156.14 29.68 89.49 Scale applied to data: s=0.216793 (maximum obs:4612682.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.013; Rsigma 0.021: data 428 -> merged 104 With outlier rejection... Rint 0.012; Rsigma 0.022: data 426 -> merged 104 Rejected total: 2, method kkm 2, method Blessing 0 Completeness direct cell (a, b, c) = (8.382, 8.382, 8.382), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586883, 4.839560 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.71 8 10 3.13 80.00 25 1.61 - 1.21 10 10 3.80 100.00 38 1.17 - 1.02 10 10 5.30 100.00 53 0.99 - 0.89 10 10 4.70 100.00 47 0.88 - 0.81 10 10 4.80 100.00 48 0.81 - 0.74 10 10 4.40 100.00 44 0.73 - 0.71 10 10 4.30 100.00 43 0.70 - 0.66 10 10 4.10 100.00 41 0.66 - 0.64 10 10 3.30 100.00 33 0.63 - 0.60 12 12 3.67 100.00 44 --------------------------------------------------------------- 5.93 - 0.60 100 102 4.16 98.04 416 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:20:00 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929479 5.923028 5.932701 59.9878 90.0320 59.9914 378 Reflections read from file xs1714a.hkl; mean (I/sigma) = 31.46 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 187 181 192 190 280 254 254 378 N (int>3sigma) = 0 167 181 172 168 260 226 225 338 Mean intensity = 0.0 60.6 24.4 59.6 55.8 48.6 71.7 61.3 64.2 Mean int/sigma = 0.0 31.0 29.9 31.8 31.2 30.9 31.4 29.8 31.5 Lattice type: P chosen Volume: 147.24 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.923 5.925 5.926 119.92 90.10 119.94 Niggli form: a.a = 35.082 b.b = 35.111 c.c = 35.117 b.c = -17.515 a.c = -0.059 a.b = -17.517 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.075 CUBIC F-lattice R(int) = 0.330 [ 230] Vol = 589.0 Cell: 8.371 8.390 8.385 90.03 89.97 90.01 Volume: 588.98 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.075 RHOMBOHEDRAL R-lattice R(int) = 0.340 [ 119] Vol = 441.7 Cell: 5.925 5.923 14.525 89.91 90.11 119.94 Volume: 441.73 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.075 RHOMBOHEDRAL R-lattice R(int) = 0.374 [ 24] Vol = 441.7 Trigonal Cell: 5.925 5.923 14.525 89.91 90.11 119.94 Volume: 441.73 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.051 TETRAGONAL I-lattice R(int) = 0.350 [ 150] Vol = 294.5 Cell: 5.929 5.933 8.371 89.97 89.99 90.03 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.055 TETRAGONAL I-lattice R(int) = 0.350 [ 150] Vol = 294.5 Cell: 5.929 5.933 8.371 89.97 89.99 90.03 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.048 ORTHORHOMBIC I-lattice R(int) = 0.358 [ 197] Vol = 294.5 Cell: 5.929 8.371 5.933 89.97 89.97 90.01 Volume: 294.49 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.030 MONOCLINIC I-lattice R(int) = 0.308 [ 107] Vol = 294.5 Cell: 8.371 5.929 5.933 90.03 90.03 90.01 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.063 MONOCLINIC I-lattice R(int) = 0.260 [ 41] Vol = 294.5 Cell: 5.926 5.923 8.390 90.01 90.03 89.90 Volume: 294.49 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.022 MONOCLINIC C-lattice R(int) = 0.257 [ 31] Vol = 294.5 Cell: 8.371 8.390 5.923 90.01 134.94 90.01 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.423 [ 3] Vol = 147.2 Cell: 5.923 5.925 5.926 119.92 90.10 119.94 Volume: 147.24 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 181 0 254 256 378 N (int>3sigma) = 0 0 0 0 181 0 226 232 338 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 71.7 65.0 64.2 Mean int/sigma = 0.0 0.0 0.0 0.0 29.9 0.0 31.4 32.5 31.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.334 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 6 6 36 79 N I>3s 6 6 27 79 0.6 0.6 0.6 27.0 10.7 10.7 5.4 32.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.330 213 Fd-3m 1 1 227 C N N N N 37 2284 0.394 249 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371451 8.390170 8.385486 90.0311 89.9720 90.0125 ZERR 1.00 0.009950 0.004283 0.000723 0.0059 0.0320 0.0074 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4605282- 670271 92 90 26 3.5 1462959.18 69.69 0.010 0.011 618367- 129834 129 129 26 5.0 254213.89 33.46 0.015 0.019 126345- 12748 99 99 26 3.8 90933.98 13.63 0.024 0.028 6532- 2177 108 108 26 4.2 3898.65 3.48 0.124 0.136 ------------------------------------------------------------------------------------------- 4605282- 2177 428 426 104 4.1 408177.08 28.90 0.012 0.013 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 116 114 27 4.2 635607.75 48.18 0.012 0.013 0.012 0.99-0.78 122 122 26 4.7 429050.10 28.40 0.011 0.012 0.021 0.77-0.65 115 115 28 4.1 300162.98 19.73 0.011 0.012 0.032 0.65-0.59 75 75 23 3.3 194150.64 14.46 0.020 0.023 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 428 426 104 4.1 408177.08 28.90 0.012 0.013 0.022 inf-0.60 416 414 99 4.2 414105.88 29.37 0.012 0.013 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 114 29 27 93.1 4.2 635607.75 103.08 0.012 0.006 0.99-0.78 122 26 26 100.0 4.7 429050.10 65.82 0.011 0.010 0.77-0.65 115 28 28 100.0 4.1 300162.98 43.74 0.011 0.016 0.65-0.59 75 26 23 88.5 3.3 194150.64 27.75 0.020 0.025 -------------------------------------------------------------------------------------------- inf-0.59 426 109 104 95.4 4.1 408177.08 63.13 0.012 0.011 inf-0.60 414 101 99 98.0 4.2 414105.88 64.36 0.012 0.010 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:27:03 2018) ID: 2932; threads 39; handles 876; mem 517316.00 (1237820.00)kB; time: 1w 4d 22h 32m 34s MEMORY INFO: Memory PF:244.0, Ph:425.0, V:1208.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:505.2,peak PF: 697.1, WS: 296.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:246.0, Ph:425.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.0,peak PF: 697.1, WS: 298.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:27:03 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000030 0.000041 0.000022 ) -0.068858 -0.065594 -0.010716 ( 0.000032 0.000043 0.000023 ) 0.109112 -0.153091 0.115835 ( 0.000030 0.000041 0.000022 ) 5.91502 ( 0.00207 ) 5.91640 ( 0.00211 ) 5.92265 ( 0.00146 ) 60.05206 ( 0.03175 ) 89.98756 ( 0.02430 ) 60.01743 ( 0.03690 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:27:04 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000030 0.000041 0.000022 ) -0.068858 -0.065594 -0.010716 ( 0.000032 0.000043 0.000023 ) 0.109112 -0.153091 0.115835 ( 0.000030 0.000041 0.000022 ) M - matrix: 0.021485 -0.014354 0.007180 ( 0.000009 0.000008 0.000005 ) -0.014354 0.028716 -0.014348 ( 0.000008 0.000014 0.000007 ) 0.007180 -0.014348 0.021463 ( 0.000005 0.000007 0.000006 ) unit cell: 5.915(2) 5.916(2) 5.9227(15) 60.05(3) 89.99(2) 60.02(4) V = 146.73(7) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb PROFFITPEAK info: 1458 peaks in the peak location table UB fit with 575 obs out of 627 (total:628,skipped:1) (91.71%) UB - matrix: -0.070210 0.030798 0.088685 ( 0.000057 0.000073 0.000039 ) -0.068026 -0.066097 -0.010706 ( 0.000065 0.000083 0.000045 ) 0.109090 -0.153012 0.116286 ( 0.000087 0.000112 0.000060 ) M - matrix: 0.021458 -0.014358 0.007187 ( 0.000022 0.000020 0.000014 ) -0.014358 0.028730 -0.014354 ( 0.000020 0.000036 0.000018 ) 0.007187 -0.014354 0.021502 ( 0.000014 0.000018 0.000016 ) unit cell: 5.935(4) 5.921(4) 5.925(3) 60.03(6) 90.06(5) 59.97(7) V = 147.16(14) UB fit with 575 obs out of 627 (total:628,skipped:1) (91.71%) UB - matrix: -0.070210 0.030798 0.088685 ( 0.000057 0.000073 0.000039 ) -0.068026 -0.066097 -0.010706 ( 0.000065 0.000083 0.000045 ) 0.109090 -0.153012 0.116286 ( 0.000087 0.000112 0.000060 ) M - matrix: 0.021458 -0.014358 0.007187 ( 0.000022 0.000020 0.000014 ) -0.014358 0.028730 -0.014354 ( 0.000020 0.000036 0.000018 ) 0.007187 -0.014354 0.021502 ( 0.000014 0.000018 0.000016 ) unit cell: 5.935(4) 5.921(4) 5.925(3) 60.03(6) 90.06(5) 59.97(7) V = 147.16(14) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070163 0.030657 0.088525 ( 0.000061 0.000078 0.000042 ) -0.068081 -0.065864 -0.010675 ( 0.000060 0.000076 0.000041 ) 0.108953 -0.152744 0.115923 ( 0.000079 0.000100 0.000054 ) M - matrix: 0.021429 -0.014309 0.007146 ( 0.000021 0.000018 0.000013 ) -0.014309 0.028609 -0.014290 ( 0.000018 0.000033 0.000016 ) 0.007146 -0.014290 0.021389 ( 0.000013 0.000016 0.000015 ) UB fit with 580 obs out of 627 (total:628,skipped:1) (92.50%) unit cell: 5.937(4) 5.934(4) 5.942(3) 59.99(6) 90.00(5) 59.97(7) V = 147.94(14) UB fit with 580 obs out of 627 (total:628,skipped:1) (92.50%) UB - matrix: -0.070163 0.030657 0.088525 ( 0.000061 0.000078 0.000042 ) -0.068081 -0.065864 -0.010675 ( 0.000060 0.000076 0.000041 ) 0.108954 -0.152745 0.115924 ( 0.000079 0.000100 0.000054 ) M - matrix: 0.021429 -0.014309 0.007146 ( 0.000021 0.000018 0.000013 ) -0.014309 0.028609 -0.014290 ( 0.000018 0.000033 0.000016 ) 0.007146 -0.014290 0.021389 ( 0.000013 0.000016 0.000015 ) unit cell: 5.937(4) 5.934(4) 5.942(3) 59.99(6) 90.00(5) 59.97(7) V = 147.93(14) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 628 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Run 1 Omega scan: (-107.000 - -7.000,100 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 755 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070163 0.030657 0.088525 ( 0.000061 0.000078 0.000042 ) -0.068081 -0.065864 -0.010675 ( 0.000060 0.000076 0.000041 ) 0.108954 -0.152745 0.115924 ( 0.000079 0.000100 0.000054 ) M - matrix: 0.021429 -0.014309 0.007146 ( 0.000021 0.000018 0.000013 ) -0.014309 0.028609 -0.014290 ( 0.000018 0.000033 0.000016 ) 0.007146 -0.014290 0.021389 ( 0.000013 0.000016 0.000015 ) UB fit with 580 obs out of 627 (total:628,skipped:1) (92.50%) unit cell: 5.937(4) 5.934(4) 5.942(3) 59.99(6) 90.00(5) 59.97(7) V = 147.93(14) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 627 (total:628,skipped:1) (92.50%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb 7 of 411 peaks identified as outliers and rejected 404 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 404 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 404 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 40 | 0.978 ( 0.162) | 1.284 ( 0.619) | 1.748 ( 2.446) | 1.33- 1.09 | 40 | 1.056 ( 0.125) | 1.074 ( 0.158) | 1.089 ( 0.469) | 1.09- 0.96 | 40 | 1.069 ( 0.106) | 1.089 ( 0.135) | 1.118 ( 0.473) | 0.96- 0.86 | 40 | 1.077 ( 0.113) | 1.056 ( 0.141) | 1.116 ( 0.370) | 0.86- 0.81 | 40 | 1.114 ( 0.102) | 1.042 ( 0.131) | 1.352 ( 0.504) | 0.81- 0.73 | 40 | 1.101 ( 0.080) | 0.991 ( 0.127) | 1.307 ( 0.491) | 0.73- 0.70 | 40 | 1.092 ( 0.082) | 0.937 ( 0.103) | 1.382 ( 0.500) | 0.70- 0.67 | 40 | 1.094 ( 0.058) | 0.884 ( 0.058) | 1.422 ( 0.506) | 0.67- 0.63 | 40 | 1.076 ( 0.066) | 0.868 ( 0.064) | 1.465 ( 0.604) | 0.63- 0.59 | 44 | 1.029 ( 0.078) | 0.809 ( 0.035) | 1.274 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 404 | 1.068 ( 0.108) | 1.001 ( 0.258) | 1.327 ( 0.922) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) UB - matrix: -0.070020 0.030455 0.088670 ( 0.000027 0.000029 0.000016 ) -0.068395 -0.065738 -0.010696 ( 0.000029 0.000032 0.000017 ) 0.109070 -0.152799 0.115661 ( 0.000029 0.000031 0.000017 ) M - matrix: 0.021477 -0.014302 0.007138 ( 0.000008 0.000007 0.000005 ) -0.014302 0.028596 -0.014269 ( 0.000007 0.000011 0.000005 ) 0.007138 -0.014269 0.021354 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(16) 5.9311(17) 5.9452(11) 59.99(2) 90.006(19) 60.02(3) V = 147.79(6) OTKP changes: 404 1 1 1 OTKP changes: 404 1 1 1 OTKP changes: 404 1 1 1 UB - matrix: -0.070128 0.030635 0.088738 ( 0.000024 0.000026 0.000014 ) -0.068210 -0.065969 -0.010731 ( 0.000027 0.000029 0.000016 ) 0.109152 -0.153046 0.116026 ( 0.000026 0.000028 0.000015 ) M - matrix: 0.021485 -0.014354 0.007173 ( 0.000007 0.000006 0.000004 ) -0.014354 0.028713 -0.014331 ( 0.000006 0.000009 0.000005 ) 0.007173 -0.014331 0.021452 ( 0.000004 0.000005 0.000004 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9296(15) 5.9212(15) 5.9317(10) 60.02(2) 90.038(17) 59.98(3) V = 147.23(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - -7.000,100 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 753 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070128 0.030635 0.088738 ( 0.000024 0.000026 0.000014 ) -0.068210 -0.065969 -0.010731 ( 0.000027 0.000029 0.000016 ) 0.109152 -0.153046 0.116026 ( 0.000026 0.000028 0.000015 ) M - matrix: 0.021485 -0.014354 0.007173 ( 0.000007 0.000006 0.000004 ) -0.014354 0.028713 -0.014331 ( 0.000006 0.000009 0.000005 ) 0.007173 -0.014331 0.021452 ( 0.000004 0.000005 0.000004 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9296(15) 5.9212(15) 5.9317(10) 60.02(2) 90.038(17) 59.98(3) V = 147.23(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb 8 of 407 peaks identified as outliers and rejected 399 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 399 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 399 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 40 | 0.979 ( 0.153) | 1.274 ( 0.661) | 1.284 ( 0.759) | 1.32- 1.09 | 40 | 1.062 ( 0.117) | 1.086 ( 0.145) | 1.102 ( 0.462) | 1.09- 0.96 | 40 | 1.068 ( 0.100) | 1.091 ( 0.138) | 1.132 ( 0.483) | 0.96- 0.85 | 40 | 1.079 ( 0.109) | 1.057 ( 0.135) | 1.154 ( 0.402) | 0.85- 0.81 | 40 | 1.115 ( 0.101) | 1.041 ( 0.134) | 1.346 ( 0.479) | 0.81- 0.73 | 40 | 1.098 ( 0.079) | 0.985 ( 0.122) | 1.310 ( 0.486) | 0.73- 0.70 | 40 | 1.097 ( 0.079) | 0.944 ( 0.101) | 1.437 ( 0.476) | 0.70- 0.67 | 40 | 1.092 ( 0.059) | 0.886 ( 0.070) | 1.413 ( 0.510) | 0.67- 0.63 | 40 | 1.077 ( 0.062) | 0.869 ( 0.064) | 1.459 ( 0.592) | 0.63- 0.59 | 39 | 1.028 ( 0.075) | 0.803 ( 0.033) | 1.289 ( 0.502) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 399 | 1.070 ( 0.104) | 1.004 ( 0.268) | 1.293 ( 0.537) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-14.2 | 40 | 1.131 ( 0.047) | 1.179 ( 0.162) | 1.208 ( 0.529) | 14.2-19.7 | 40 | 1.134 ( 0.065) | 1.166 ( 0.242) | 1.304 ( 0.598) | 19.7-23.6 | 40 | 1.122 ( 0.086) | 1.176 ( 0.387) | 1.322 ( 0.538) | 23.8-28.2 | 40 | 1.108 ( 0.095) | 1.151 ( 0.445) | 1.366 ( 0.472) | 28.2-31.0 | 40 | 1.068 ( 0.095) | 0.988 ( 0.100) | 1.349 ( 0.481) | 31.1-34.5 | 40 | 1.074 ( 0.082) | 0.931 ( 0.096) | 1.290 ( 0.494) | 34.5-37.3 | 40 | 1.039 ( 0.088) | 0.885 ( 0.082) | 1.384 ( 0.578) | 37.4-39.6 | 40 | 1.021 ( 0.103) | 0.908 ( 0.208) | 1.381 ( 0.593) | 39.7-42.7 | 40 | 0.989 ( 0.107) | 0.837 ( 0.091) | 1.136 ( 0.473) | 42.7-49.7 | 39 | 1.008 ( 0.122) | 0.817 ( 0.078) | 1.184 ( 0.531) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.7 | 399 | 1.070 ( 0.104) | 1.004 ( 0.268) | 1.293 ( 0.537) | Fitted profile normalization line parameters e1 dimension: a=-0.0030 b=1.12 e2 dimension: a=-0.0108 b=1.29 e3 dimension: a=0.0061 b=0.90 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 4108 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706981 Maximum peak integral for reflections I/sig<= 10000 - raw: 8009297 lp-corr: 2344450 PROFFITPEAK - Finished at Tue Mar 27 13:27:11 2018 PROFFITMAIN - Started at Tue Mar 27 13:27:11 2018 OTKP changes: 399 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 399 1 1 1 OTKP changes: 399 1 1 1 OTKP changes: 399 1 1 1 UB - matrix: -0.070131 0.030630 0.088747 ( 0.000026 0.000028 0.000015 ) -0.068213 -0.065957 -0.010740 ( 0.000025 0.000027 0.000014 ) 0.109146 -0.153041 0.116009 ( 0.000022 0.000024 0.000013 ) M - matrix: 0.021484 -0.014353 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014353 0.028710 -0.014327 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014327 0.021450 ( 0.000004 0.000004 0.000004 ) UB fit with 399 obs out of 399 (total:399,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9316(11) 60.03(2) 90.032(17) 59.98(2) V = 147.23(5) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Run 1 Omega scan: (-107.000 - -7.000,100 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 755 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070131 0.030630 0.088747 ( 0.000026 0.000028 0.000015 ) -0.068213 -0.065957 -0.010740 ( 0.000025 0.000027 0.000014 ) 0.109146 -0.153041 0.116009 ( 0.000022 0.000024 0.000013 ) M - matrix: 0.021484 -0.014353 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014353 0.028710 -0.014327 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014327 0.021450 ( 0.000004 0.000004 0.000004 ) UB fit with 399 obs out of 399 (total:399,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9316(11) 60.03(2) 90.032(17) 59.98(2) V = 147.23(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 399 obs out of 399 (total:399,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070131 0.030630 0.088747 ( 0.000026 0.000028 0.000015 ) -0.068213 -0.065957 -0.010740 ( 0.000025 0.000027 0.000014 ) 0.109146 -0.153041 0.116009 ( 0.000022 0.000024 0.000013 ) M - matrix: 0.021484 -0.014353 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014353 0.028710 -0.014327 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014327 0.021450 ( 0.000004 0.000004 0.000004 ) UB fit with 399 obs out of 399 (total:399,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9316(11) 60.03(2) 90.032(17) 59.98(2) V = 147.23(5) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070131 0.030630 0.088747 ( 0.000026 0.000028 0.000015 ) -0.068213 -0.065957 -0.010740 ( 0.000025 0.000027 0.000014 ) 0.109146 -0.153041 0.116009 ( 0.000022 0.000024 0.000013 ) M - matrix: 0.021484 -0.014353 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014353 0.028710 -0.014327 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014327 0.021450 ( 0.000004 0.000004 0.000004 ) UB fit with 399 obs out of 399 (total:399,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9316(11) 60.03(2) 90.032(17) 59.98(2) V = 147.23(5) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 26 reflections under beam stop or inside a detector rejection region 2 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof 571 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:27:12 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - -7.000,100 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=240.0000 max=12215997.0000 PROFFIT INFO: signal sum lp corr: min=634.3988 max=2942319.4424 PROFFIT INFO: background sum: min=1310.0000 max=6867.0000 PROFFIT INFO: background sum sig2: min=673.0000 max=6478.0000 PROFFIT INFO: num of signal pixels: min=63 max=531 PROFFIT INFO: Inet: min=1015.0381 max=4707711.5000 PROFFIT INFO: sig(Inet): min=182.2551 max=47465.4219 PROFFIT INFO: Inet/sig(Inet): min=1.07 max=228.17 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 21 57 123 134 218 372 511 571 Percent 0.0 0.0 0.7 3.7 10.0 21.5 23.5 38.2 65.1 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 571 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 571 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4707712- 1273819 57 2050963.54 132.83 100.00 1270867- 735271 57 981021.80 109.75 100.00 725930- 307405 57 467603.31 102.30 100.00 301534- 183979 57 224077.48 70.38 100.00 183970- 147090 57 167316.37 55.80 100.00 147076- 104764 57 121484.42 36.44 100.00 104312- 77834 57 91482.26 30.28 100.00 77192- 5695 57 39658.42 19.05 100.00 5617- 3388 57 4273.52 5.58 96.49 3368- 1015 58 2604.29 3.91 67.24 ------------------------------------------------------------------------------------ 4707712- 1015 571 414326.22 56.54 96.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 57 686979.74 88.55 100.00 1.24- 1.03 57 663568.24 67.29 98.25 1.03- 0.90 57 477938.77 58.30 98.25 0.90- 0.82 57 502524.62 71.40 96.49 0.82- 0.75 57 374480.46 58.55 96.49 0.75- 0.70 57 371314.80 56.79 98.25 0.70- 0.64 57 323197.87 48.03 96.49 0.64- 0.59 57 328414.62 48.31 94.74 0.59- 0.54 57 214602.36 35.67 92.98 0.54- 0.42 58 203931.86 32.91 91.38 ------------------------------------------------------------------------------------ 5.27- 0.42 571 414326.22 56.54 96.32 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:27:12 2018 Sorting 571 observations 137 unique observations with > 7.00 F2/sig(F2) 571 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Maximum number of 137 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 571 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 451 observations > 7.00 F2/sig(F2) 451 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Frame #58 of 100 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.0 (Out of 451 removed 96 = 355, unique = 118) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 355 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Frame #14 of 100 skipped from refinement Frame #23 of 100 skipped from refinement Frame #58 of 100 skipped from refinement 3 frames need to be skipped from refinement, because of missing redundant and/or observable data 118 unique data precomputed (should be 118) 118 unique data with 355 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.0 (Out of 355 removed 0 = 355, unique = 118) 118 unique data precomputed (should be 118) 118 unique data with 355 observations RMS deviation of equivalent data = 0.61641 Rint = 0.47780 2 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.44638, wR= 2.51436 Trying model 1 (ne=2, no=0)... Results: Rint= 0.90079, wR= 1.38627, Acormin=-0.269, Acormax=1.130, Acor_av=0.156 F test: Probability=0.000, F= 0.240 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88801, wR= 1.63163, Acormin=-0.424, Acormax=0.840, Acor_av=0.036 F test: Probability=0.000, F= 0.244 Trying model 3 (ne=4, no=0)... Results: Rint= 0.91647, wR= 1.06601, Acormin=-0.217, Acormax=0.811, Acor_av=0.023 F test: Probability=0.000, F= 0.223 Trying model 4 (ne=4, no=1)... Results: Rint= 0.91865, wR= 1.15560, Acormin=-0.309, Acormax=0.599, Acor_av=-0.001 F test: Probability=0.000, F= 0.219 Trying model 5 (ne=4, no=3)... Results: Rint= 0.84876, wR= 1.84770, Acormin=-0.115, Acormax=0.291, Acor_av=-0.006 F test: Probability=0.000, F= 0.248 Trying model 6 (ne=6, no=0)... Results: Rint= 0.86969, wR= 1.33656, Acormin=-0.071, Acormax=0.613, Acor_av=0.001 F test: Probability=0.000, F= 0.233 Trying model 7 (ne=6, no=1)... Results: Rint= 0.86834, wR= 1.33929, Acormin=-0.136, Acormax=0.582, Acor_av=-0.001 F test: Probability=0.000, F= 0.231 Trying model 8 (ne=6, no=3)... Results: Rint= 0.78214, wR= 1.31210, Acormin=-0.095, Acormax=0.336, Acor_av=-0.000 F test: Probability=0.000, F= 0.274 Trying model 9 (ne=6, no=5)... Results: Rint= 0.62027, wR= 1.51983, Acormin=-0.024, Acormax=0.091, Acor_av=0.003 F test: Probability=0.000, F= 0.412 Trying model 10 (ne=8, no=0)... Results: Rint= 0.83764, wR= 1.59670, Acormin=-0.050, Acormax=0.425, Acor_av=0.002 F test: Probability=0.000, F= 0.231 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87649, wR= 1.64817, Acormin=-0.071, Acormax=0.385, Acor_av=0.001 F test: Probability=0.000, F= 0.207 Trying model 12 (ne=8, no=3)... Results: Rint= 0.51031, wR= 1.53134, Acormin=-0.012, Acormax=0.029, Acor_av=0.002 F test: Probability=0.000, F= 0.589 Trying model 13 (ne=8, no=5)... Results: Rint= 0.44365, wR= 1.35308, Acormin=-0.014, Acormax=0.057, Acor_av=0.003 F test: Probability=0.000, F= 0.732 Trying model 14 (ne=8, no=7)... Results: Rint= 0.35837, wR= 0.96358, Acormin=-0.017, Acormax=0.135, Acor_av=0.004 F test: Probability=0.558, F= 1.023 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.66271 There are 97 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 101 pars with 5151 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.61641 Using Levenberg-Marquardt: 0.00010 New wR= 0.54059 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.47780 with corrections 0.54863 Rint for all data: 0.66271 with corrections 0.71238 2 observations identified as outliers and rejected Cycle 2 wR= 0.53204 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.51841 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44638 with corrections 0.44149 Rint for all data: 0.66271 with corrections 0.65519 0 observations identified as outliers and rejected Cycle 3 wR= 0.51841 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.51373 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44638 with corrections 0.43529 Rint for all data: 0.66271 with corrections 0.65045 0 observations identified as outliers and rejected Cycle 4 wR= 0.51373 Using Levenberg-Marquardt: 0.10000 New wR= 0.50667 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44638 with corrections 0.43326 Rint for all data: 0.66271 with corrections 0.64886 0 observations identified as outliers and rejected Cycle 5 wR= 0.50667 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.49805 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44638 with corrections 0.42999 Rint for all data: 0.66271 with corrections 0.64771 0 observations identified as outliers and rejected Final wR= 0.49805 Final frame scales: Min= 0.4551 Max= 5.4713 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time with different frame scales initialization There are 97 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 96 pars with 4656 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.76657 Using Levenberg-Marquardt: 0.00010 New wR= 0.56953 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44638 with corrections 0.42357 Rint for all data: 0.66271 with corrections 0.64495 1 observations identified as outliers and rejected Cycle 2 wR= 0.56142 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.54550 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44479 with corrections 0.44039 Rint for all data: 0.66271 with corrections 0.66258 0 observations identified as outliers and rejected Cycle 3 wR= 0.54550 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.52584 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44479 with corrections 0.44747 Rint for all data: 0.66271 with corrections 0.66963 0 observations identified as outliers and rejected Cycle 4 wR= 0.52584 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.51780 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44479 with corrections 0.47231 Rint for all data: 0.66271 with corrections 0.68910 0 observations identified as outliers and rejected Cycle 5 wR= 0.51780 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.51624 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.44479 with corrections 0.50728 Rint for all data: 0.66271 with corrections 0.71394 0 observations identified as outliers and rejected Final wR= 0.51624 Final frame scales: Min= 1.0000 Max= 13.7879 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 63 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 62 pars with 1953 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.85035 Using Levenberg-Marquardt: 0.00010 New wR= 0.68574 There are 13 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.52696 Rint for all data: 0.66271 with corrections 0.71090 0 observations identified as outliers and rejected Cycle 2 wR= 0.59344 Using Levenberg-Marquardt: 0.00001 New wR= 0.52759 There are 13 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.50737 Rint for all data: 0.66271 with corrections 0.70679 0 observations identified as outliers and rejected Cycle 3 wR= 0.57198 Using Levenberg-Marquardt: 0.00000 New wR= 0.55992 There are 13 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.48166 Rint for all data: 0.66271 with corrections 0.68222 0 observations identified as outliers and rejected Cycle 4 wR= 0.57290 Using Levenberg-Marquardt: 0.00000 New wR= 0.54642 There are 13 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.46963 Rint for all data: 0.66271 with corrections 0.67448 0 observations identified as outliers and rejected Cycle 5 wR= 0.57085 Using Levenberg-Marquardt: 0.00000 New wR= 0.55061 There are 13 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.47478 Rint for all data: 0.66271 with corrections 0.67830 0 observations identified as outliers and rejected Final wR= 0.55061 Final frame scales: Min= 0.1840 Max= 2.3185 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 61 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 60 pars with 1830 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.17348 Using Levenberg-Marquardt: 0.00010 New wR= 0.60650 There are 14 clusters with unrefined scales (size 1-10) Rint for refined data: 0.44479 with corrections 0.43962 Rint for all data: 0.66271 with corrections 0.65935 1 observations identified as outliers and rejected Cycle 2 wR= 0.58444 Using Levenberg-Marquardt: 0.00001 New wR= 0.53556 There are 14 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.39771 Rint for all data: 0.66271 with corrections 0.63009 0 observations identified as outliers and rejected Cycle 3 wR= 0.55845 Using Levenberg-Marquardt: 0.00000 New wR= 0.53290 There are 14 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.45893 Rint for all data: 0.66271 with corrections 0.70145 0 observations identified as outliers and rejected Cycle 4 wR= 0.55905 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.55093 There are 14 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.43533 Rint for all data: 0.66271 with corrections 0.67688 0 observations identified as outliers and rejected Cycle 5 wR= 0.55266 Using Levenberg-Marquardt: 0.10000 New wR= 0.54716 There are 14 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.42613 Rint for all data: 0.66271 with corrections 0.66451 0 observations identified as outliers and rejected Final wR= 0.54716 Final frame scales: Min= 0.1304 Max= 2.4936 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 58 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 57 pars with 1653 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.57348 Using Levenberg-Marquardt: 0.00010 New wR= 0.59276 There are 15 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.42247 Rint for all data: 0.66271 with corrections 0.65478 0 observations identified as outliers and rejected Cycle 2 wR= 0.58402 Using Levenberg-Marquardt: 0.00001 New wR= 0.55754 There are 15 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.40234 Rint for all data: 0.66271 with corrections 0.63198 0 observations identified as outliers and rejected Cycle 3 wR= 0.56459 Using Levenberg-Marquardt: 0.00000 New wR= 0.55583 There are 15 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.41297 Rint for all data: 0.66271 with corrections 0.63964 0 observations identified as outliers and rejected Cycle 4 wR= 0.56464 Using Levenberg-Marquardt: 0.00000 New wR= 0.55230 There are 15 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.41110 Rint for all data: 0.66271 with corrections 0.63852 0 observations identified as outliers and rejected Cycle 5 wR= 0.56130 Using Levenberg-Marquardt: 0.00000 New wR= 0.55361 There are 15 clusters with unrefined scales (size 1-10) Rint for refined data: 0.43965 with corrections 0.42026 Rint for all data: 0.66271 with corrections 0.64570 0 observations identified as outliers and rejected Final wR= 0.55361 Final frame scales: Min= 0.2058 Max= 2.0058 1 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=1067.9172 max=4808304.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=134.3454 max=75437.2891 PROFFIT INFO: 4 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:1/100 567 reflections read from tmp file 468 reflections are rejected (345 as outliers, 123 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 38 5 2 Initial Chi^2= 0.94946 Cycle 1, Chi^2= 0.91579 Current error model SIG(F2)^2 = 203.82*I_RAW + 16.48*I_BACK+(0.03716*)^2 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 0.90142 Current error model SIG(F2)^2 = 296.58*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 267.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 267.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4808305- 1213180 56 2076375.14 86.86 100.00 1196136- 717929 56 951446.67 48.68 100.00 711960- 305121 56 468249.85 43.64 100.00 300593- 190173 56 237101.13 28.45 100.00 189638- 148518 56 169861.21 23.35 100.00 148064- 101124 56 123101.49 18.37 100.00 100741- 70165 56 84897.02 12.70 100.00 70154- 6455 56 40368.25 10.14 89.29 6420- 3260 56 4424.09 3.39 44.64 3244- 1068 63 2400.89 2.96 38.10 ------------------------------------------------------------------------------------ 4808305- 1068 567 410718.60 27.55 86.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 56 671232.57 59.30 98.21 1.28- 1.03 56 694907.27 39.92 94.64 1.03- 0.92 56 527079.36 31.40 91.07 0.92- 0.82 56 467991.60 29.22 83.93 0.82- 0.75 56 351693.79 24.39 83.93 0.75- 0.70 56 381776.36 23.44 89.29 0.70- 0.64 56 312273.50 20.93 85.71 0.64- 0.59 56 316163.93 19.39 83.93 0.59- 0.55 56 200989.10 14.90 76.79 0.54- 0.42 63 208371.88 14.24 79.37 ------------------------------------------------------------------------------------ 5.27- 0.42 567 410718.60 27.55 86.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 56 671232.57 59.30 98.21 5.27- 1.03 112 683069.92 49.61 96.43 5.27- 0.92 168 631073.07 43.54 94.64 5.27- 0.82 224 590302.70 39.96 91.96 5.27- 0.75 280 542580.92 36.84 90.36 5.27- 0.70 336 515780.16 34.61 90.18 5.27- 0.64 392 486707.78 32.66 89.54 5.27- 0.59 448 465389.80 31.00 88.84 5.27- 0.55 504 436011.94 29.21 87.50 5.27- 0.42 567 410718.60 27.55 86.60 ------------------------------------------------------------------------------------ 5.27- 0.42 567 410718.60 27.55 86.60 Scale applied to data: s=0.207973 (maximum obs:4808304.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.637; Rsigma 0.024: data 567 -> merged 241 With outlier rejection... Rint 0.502; Rsigma 0.024: data 495 -> merged 241 Rejected total: 72, method kkm 70, method Blessing 2 Completeness direct cell (a, b, c) = (5.280, 5.280, 5.280), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.425509, 5.280432 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.46 15 15 1.93 100.00 29 1.46 - 1.13 15 15 3.33 100.00 50 1.08 - 0.96 15 15 3.60 100.00 54 0.96 - 0.86 15 15 3.20 100.00 48 0.86 - 0.79 15 15 2.60 100.00 39 0.79 - 0.73 15 15 2.67 100.00 40 0.73 - 0.69 14 15 2.00 93.33 28 0.69 - 0.65 15 15 1.80 100.00 27 0.65 - 0.64 14 15 1.79 93.33 25 0.63 - 0.60 21 21 1.62 100.00 34 --------------------------------------------------------------- 5.93 - 0.60 154 156 2.43 98.72 374 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:27:13 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929628 5.921422 5.931558 60.0255 90.0319 59.9779 495 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.90 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 246 254 244 256 372 330 333 495 N (int>3sigma) = 0 211 254 209 216 337 284 285 425 Mean intensity = 0.0 68.4 34.2 69.5 77.8 57.1 82.4 77.7 78.9 Mean int/sigma = 0.0 23.6 22.3 24.3 26.4 23.4 26.2 26.4 25.9 Lattice type: P chosen Volume: 147.23 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.921 5.924 5.928 119.93 90.09 119.92 Niggli form: a.a = 35.063 b.b = 35.088 c.c = 35.136 b.c = -17.521 a.c = -0.052 a.b = -17.496 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.217 [ 344] Vol = 588.9 Cell: 8.372 8.389 8.385 90.02 89.94 90.05 Volume: 588.94 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.211 [ 221] Vol = 441.7 Cell: 5.924 5.921 14.529 89.94 90.08 119.92 Volume: 441.70 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.242 [ 56] Vol = 441.7 Trigonal Cell: 5.924 5.921 14.529 89.94 90.08 119.92 Volume: 441.70 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.183 [ 195] Vol = 294.5 Cell: 5.930 5.932 8.372 89.92 89.99 90.03 Volume: 294.47 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.093 TETRAGONAL I-lattice R(int) = 0.183 [ 195] Vol = 294.5 Cell: 5.930 5.932 8.372 89.92 89.99 90.03 Volume: 294.47 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.083 ORTHORHOMBIC I-lattice R(int) = 0.175 [ 250] Vol = 294.5 Cell: 5.930 8.372 5.932 89.92 89.97 90.01 Volume: 294.47 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.161 [ 145] Vol = 294.5 Cell: 8.372 5.930 5.932 90.03 90.08 90.01 Volume: 294.47 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.064 MONOCLINIC I-lattice R(int) = 0.220 [ 114] Vol = 294.5 Cell: 5.928 5.921 8.389 89.98 90.05 89.91 Volume: 294.47 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.064 MONOCLINIC C-lattice R(int) = 0.272 [ 56] Vol = 294.5 Cell: 8.372 8.389 5.921 89.98 134.93 90.05 Volume: 294.47 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.280 [ 4] Vol = 147.2 Cell: 5.921 5.924 5.928 119.93 90.09 119.92 Volume: 147.23 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 254 0 330 333 495 N (int>3sigma) = 0 0 0 0 254 0 284 289 425 Mean intensity = 0.0 0.0 0.0 0.0 34.2 0.0 82.4 79.1 78.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.3 0.0 26.2 26.2 25.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.204 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 37 112 N I>3s 7 7 27 112 1.0 1.0 0.8 39.9 7.0 7.0 4.0 27.0 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.217 326 Fd-3m 1 1 227 C N N N N 37 2284 0.225 363 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.372260 8.389460 8.384790 90.0186 89.9402 90.0506 ZERR 1.00 0.006827 0.003024 0.000490 0.0036 0.0221 0.0042 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4104631- 865759 67 60 26 2.3 1518674.14 65.65 0.454 0.386 853885- 592315 63 52 26 2.0 698541.42 37.97 0.532 0.456 578168- 362569 74 62 26 2.4 350942.80 25.57 0.838 0.809 362407- 232488 79 66 26 2.5 229854.34 26.31 0.498 0.561 223143- 131305 83 67 26 2.6 164829.52 24.05 0.292 0.241 130927- 98335 53 49 26 1.9 113179.77 14.54 0.319 0.252 97997- 78426 46 44 26 1.7 93191.89 13.29 0.533 0.450 77921- 48658 48 42 26 1.6 57150.55 10.58 0.139 0.139 34133- 1251 54 53 33 1.6 8147.64 4.43 0.351 0.317 ------------------------------------------------------------------------------------------- 4104631- 1251 567 495 241 2.1 379586.71 25.90 0.502 0.452 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.18 75 62 27 2.3 727388.90 55.02 0.450 0.400 0.012 1.15-0.89 117 104 27 3.9 480592.95 30.71 0.643 0.624 0.021 0.88-0.75 80 64 26 2.5 373341.73 24.30 0.317 0.218 0.024 0.75-0.69 74 62 26 2.4 318249.16 21.47 0.434 0.394 0.029 0.69-0.64 56 46 26 1.8 296344.63 19.20 0.388 0.389 0.033 0.64-0.59 47 42 26 1.6 305143.73 19.55 0.503 0.503 0.033 0.59-0.56 43 40 26 1.5 154990.98 12.62 0.730 0.730 0.048 0.56-0.53 36 36 27 1.3 271597.83 17.82 0.378 0.378 0.038 0.52-0.43 39 39 30 1.3 173468.51 12.34 0.845 0.845 0.046 ------------------------------------------------------------------------------------------------------ inf-0.43 567 495 241 2.1 379586.71 25.90 0.502 0.452 0.024 inf-0.60 442 374 154 2.4 434591.01 29.50 0.493 0.433 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.18 62 27 27 100.0 2.3 727388.90 90.74 0.450 0.009 1.15-0.89 104 27 27 100.0 3.9 480592.95 67.03 0.643 0.014 0.88-0.75 64 26 26 100.0 2.5 373341.73 41.03 0.317 0.016 0.75-0.69 62 27 26 96.3 2.4 318249.16 37.14 0.434 0.019 0.69-0.64 46 27 26 96.3 1.8 296344.63 26.80 0.388 0.024 0.64-0.59 42 26 26 100.0 1.6 305143.73 27.82 0.503 0.025 0.59-0.56 40 32 26 81.3 1.5 154990.98 18.26 0.730 0.037 0.56-0.53 36 34 27 79.4 1.3 271597.83 22.38 0.378 0.030 0.52-0.43 39 179 30 16.8 1.3 173468.51 16.16 0.845 0.037 -------------------------------------------------------------------------------------------- inf-0.43 495 407 241 59.2 2.1 379586.71 44.63 0.502 0.018 inf-0.60 374 156 154 98.7 2.4 434591.01 52.75 0.493 0.016 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.015315 -0.079439 0.024623 ( 0.000014 0.000011 0.000013 ) 0.032978 -0.028737 -0.072455 ( 0.000013 0.000011 0.000013 ) 0.076521 -0.003432 0.036057 ( 0.000012 0.000009 0.000011 ) M - matrix: 0.007178 0.000006 -0.000007 ( 0.000002 0.000001 0.000001 ) 0.000006 0.007148 0.000002 ( 0.000001 0.000002 0.000001 ) -0.000007 0.000002 0.007156 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.015315 -0.079439 0.024623 ( 0.000014 0.000011 0.000013 ) 0.032978 -0.028737 -0.072455 ( 0.000013 0.000011 0.000013 ) 0.076521 -0.003432 0.036057 ( 0.000012 0.000009 0.000011 ) M - matrix: 0.007154 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007154 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007154 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3723(12) 8.3895(11) 8.3848(12) 90.019(12) 89.940(12) 90.051(12) V = 588.94(14) unit cell: 8.3822(4) 8.3822(4) 8.3822(4) 90.0 90.0 90.0 V = 588.94(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - -7.000,100 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=240.0000 max=12215997.0000 PROFFIT INFO: signal sum lp corr: min=634.3988 max=2942319.4424 PROFFIT INFO: background sum: min=1310.0000 max=6867.0000 PROFFIT INFO: background sum sig2: min=673.0000 max=6478.0000 PROFFIT INFO: num of signal pixels: min=63 max=531 PROFFIT INFO: Inet: min=1015.0381 max=4707711.5000 PROFFIT INFO: sig(Inet): min=182.2551 max=47465.4219 PROFFIT INFO: Inet/sig(Inet): min=1.07 max=228.17 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 42 114 246 268 436 744 1022 1142 Percent 0.0 0.0 0.7 3.7 10.0 21.5 23.5 38.2 65.1 89.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 571 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 571 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4707712- 1273819 57 2050963.54 132.83 100.00 1270867- 735271 57 981021.80 109.75 100.00 725930- 307405 57 467603.31 102.30 100.00 301534- 183979 57 224077.48 70.38 100.00 183970- 147090 57 167316.37 55.80 100.00 147076- 104764 57 121484.42 36.44 100.00 104312- 77834 57 91482.26 30.28 100.00 77192- 5695 57 39658.42 19.05 100.00 5617- 3388 57 4273.52 5.58 96.49 3368- 1015 58 2604.29 3.91 67.24 ------------------------------------------------------------------------------------ 4707712- 1015 571 414326.22 56.54 96.32 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 57 675966.47 86.99 100.00 1.32- 1.09 57 898724.90 78.75 100.00 1.09- 0.96 57 437289.63 72.99 100.00 0.96- 0.85 57 486450.14 71.17 98.25 0.85- 0.80 57 466142.13 67.54 100.00 0.80- 0.73 57 253809.00 42.22 100.00 0.73- 0.70 57 257778.59 39.43 84.21 0.70- 0.65 57 313510.45 46.83 96.49 0.65- 0.63 57 184795.28 31.13 89.47 0.62- 0.59 58 173028.91 28.81 94.83 ------------------------------------------------------------------------------------ 4.83- 0.59 571 414326.22 56.54 96.32 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:27:13 2018 Sorting 571 observations 76 unique observations with > 7.00 F2/sig(F2) 571 observations in 1 runs Run # start # end # total # 1 0 99 100 Total number of frames 100 Maximum number of 76 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 571 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 451 observations > 7.00 F2/sig(F2) 451 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 Removing 'redundancy=1' reflections Average redundancy: 5.8 (Out of 451 removed 9 = 442, unique = 76) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 442 observations in 1 runs Run # start # end # total # 1 0 49 50 Total number of frames 50 76 unique data precomputed (should be 76) 76 unique data with 442 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.8 (Out of 442 removed 0 = 442, unique = 76) 76 unique data precomputed (should be 76) 76 unique data with 442 observations RMS deviation of equivalent data = 0.07146 Rint = 0.06045 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.05628, wR= 0.07394 Trying model 1 (ne=2, no=0)... Results: Rint= 0.02991, wR= 0.03950, Acormin=0.814, Acormax=1.117, Acor_av=0.893 F test: Probability=1.000, F= 3.492 Trying model 2 (ne=2, no=1)... Results: Rint= 0.02471, wR= 0.03178, Acormin=0.818, Acormax=1.217, Acor_av=0.918 F test: Probability=1.000, F= 1.453 Trying model 3 (ne=4, no=0)... Results: Rint= 0.01852, wR= 0.02600, Acormin=0.819, Acormax=1.274, Acor_av=0.967 F test: Probability=1.000, F= 1.750 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01671, wR= 0.02361, Acormin=0.843, Acormax=1.272, Acor_av=0.976 F test: Probability=0.967, F= 1.219 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01512, wR= 0.02083, Acormin=0.855, Acormax=1.320, Acor_av=0.980 F test: Probability=0.952, F= 1.197 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01558, wR= 0.02147, Acormin=0.849, Acormax=1.317, Acor_av=0.979 F test: Probability=0.000, F= 0.934 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01375, wR= 0.01926, Acormin=0.854, Acormax=1.314, Acor_av=0.981 F test: Probability=0.943, F= 1.188 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01361, wR= 0.01852, Acormin=0.852, Acormax=1.315, Acor_av=0.982 F test: Probability=0.941, F= 1.187 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01287, wR= 0.01739, Acormin=0.856, Acormax=1.349, Acor_av=0.984 F test: Probability=0.988, F= 1.282 Final absorption model (ne=6, no=5): Rint= 0.01287, Acormin=0.856, Acormax=1.349, Acor_av=0.984 Combined refinement in use Rint: 0.06061 There are 50 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 97 pars with 4753 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.07146 Using Levenberg-Marquardt: 0.00010 New wR= 0.01562 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06045 with corrections 0.01142 Rint for all data: 0.06061 with corrections 0.01165 0 observations identified as outliers and rejected Cycle 2 wR= 0.01562 Using Levenberg-Marquardt: 0.00001 New wR= 0.01519 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06045 with corrections 0.01148 Rint for all data: 0.06061 with corrections 0.01171 0 observations identified as outliers and rejected Cycle 3 wR= 0.01519 Using Levenberg-Marquardt: 0.00000 New wR= 0.01491 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06045 with corrections 0.01127 Rint for all data: 0.06061 with corrections 0.01150 0 observations identified as outliers and rejected Cycle 4 wR= 0.01491 Using Levenberg-Marquardt: 0.00000 New wR= 0.01466 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06045 with corrections 0.01101 Rint for all data: 0.06061 with corrections 0.01124 0 observations identified as outliers and rejected Cycle 5 wR= 0.01466 Using Levenberg-Marquardt: 0.00000 New wR= 0.01461 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06045 with corrections 0.01100 Rint for all data: 0.06061 with corrections 0.01123 0 observations identified as outliers and rejected Final wR= 0.01461 Final frame scales: Min= 0.9361 Max= 1.0058 Final absorption correction factors: Amin= 0.6773 Amax= 1.2981 PROFFIT INFO: Inet (after scale3 abspack): min=981.6230 max=4801481.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=185.2990 max=46578.3984 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:1/100 571 reflections read from tmp file 15 reflections are rejected (6 as outliers, 9 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 13 9 13 18 10 10 6 7 11 Initial Chi^2= 0.23153 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.02511 Current error model SIG(F2)^2 = 104.97*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 107.61*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 107.61*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4801482- 1247270 57 2081748.53 145.42 100.00 1236812- 719036 57 963836.39 69.26 100.00 708807- 320312 57 472917.22 70.91 100.00 319501- 187796 57 224371.69 46.34 100.00 187324- 148846 57 167549.67 33.93 100.00 147692- 104088 57 118085.64 23.91 100.00 104085- 80000 57 92093.20 19.78 100.00 78470- 5507 57 39312.21 13.42 100.00 5465- 3270 57 4230.76 5.17 100.00 3248- 982 58 2603.24 4.28 93.10 ------------------------------------------------------------------------------------ 4801482- 982 571 415949.69 43.17 99.30 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 57 693507.66 88.71 100.00 1.32- 1.09 57 917022.91 83.00 100.00 1.09- 0.96 57 446931.34 48.45 100.00 0.96- 0.85 57 478909.10 45.56 100.00 0.85- 0.80 57 461695.81 43.23 100.00 0.80- 0.73 57 251344.54 27.53 100.00 0.73- 0.70 57 254501.98 25.79 94.74 0.70- 0.65 57 309459.93 30.19 100.00 0.65- 0.63 57 181691.52 20.56 98.25 0.62- 0.59 58 168768.58 19.15 100.00 ------------------------------------------------------------------------------------ 4.83- 0.59 571 415949.69 43.17 99.30 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 57 693507.66 88.71 100.00 4.83- 1.09 114 805265.29 85.86 100.00 4.83- 0.96 171 685820.64 73.39 100.00 4.83- 0.85 228 634092.75 66.43 100.00 4.83- 0.80 285 599613.36 61.79 100.00 4.83- 0.73 342 541568.56 56.08 100.00 4.83- 0.70 399 500559.05 51.75 99.25 4.83- 0.65 456 476671.66 49.06 99.34 4.83- 0.63 513 443896.09 45.89 99.22 4.83- 0.59 571 415949.69 43.17 99.30 ------------------------------------------------------------------------------------ 4.83- 0.59 571 415949.69 43.17 99.30 Scale applied to data: s=0.208269 (maximum obs:4801481.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.011; Rsigma 0.015: data 571 -> merged 106 With outlier rejection... Rint 0.011; Rsigma 0.015: data 568 -> merged 106 Rejected total: 3, method kkm 3, method Blessing 0 Completeness direct cell (a, b, c) = (8.382, 8.382, 8.382), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586869, 4.839444 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.71 9 10 3.11 90.00 28 1.61 - 1.21 10 10 5.10 100.00 51 1.17 - 1.02 10 10 6.80 100.00 68 0.99 - 0.89 10 10 6.50 100.00 65 0.88 - 0.81 10 10 6.50 100.00 65 0.81 - 0.74 10 10 5.40 100.00 54 0.73 - 0.71 10 10 6.40 100.00 64 0.70 - 0.66 10 10 5.10 100.00 51 0.66 - 0.64 10 10 4.90 100.00 49 0.63 - 0.60 12 12 4.92 100.00 59 --------------------------------------------------------------- 5.93 - 0.60 101 102 5.49 99.02 554 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:27:13 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929628 5.921422 5.931558 60.0255 90.0319 59.9779 495 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.90 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 246 254 244 256 372 330 333 495 N (int>3sigma) = 0 211 254 209 216 337 284 285 425 Mean intensity = 0.0 68.4 34.2 69.5 77.8 57.1 82.4 77.7 78.9 Mean int/sigma = 0.0 23.6 22.3 24.3 26.4 23.4 26.2 26.4 25.9 Lattice type: P chosen Volume: 147.23 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.921 5.924 5.928 119.93 90.09 119.92 Niggli form: a.a = 35.063 b.b = 35.088 c.c = 35.136 b.c = -17.521 a.c = -0.052 a.b = -17.496 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.106 CUBIC F-lattice R(int) = 0.217 [ 344] Vol = 588.9 Cell: 8.372 8.389 8.385 90.02 89.94 90.05 Volume: 588.94 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.211 [ 221] Vol = 441.7 Cell: 5.924 5.921 14.529 89.94 90.08 119.92 Volume: 441.70 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.095 RHOMBOHEDRAL R-lattice R(int) = 0.242 [ 56] Vol = 441.7 Trigonal Cell: 5.924 5.921 14.529 89.94 90.08 119.92 Volume: 441.70 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.118 TETRAGONAL I-lattice R(int) = 0.183 [ 195] Vol = 294.5 Cell: 5.930 5.932 8.372 89.92 89.99 90.03 Volume: 294.47 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.093 TETRAGONAL I-lattice R(int) = 0.183 [ 195] Vol = 294.5 Cell: 5.930 5.932 8.372 89.92 89.99 90.03 Volume: 294.47 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.083 ORTHORHOMBIC I-lattice R(int) = 0.175 [ 250] Vol = 294.5 Cell: 5.930 8.372 5.932 89.92 89.97 90.01 Volume: 294.47 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.026 MONOCLINIC I-lattice R(int) = 0.161 [ 145] Vol = 294.5 Cell: 8.372 5.930 5.932 90.03 90.08 90.01 Volume: 294.47 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.064 MONOCLINIC I-lattice R(int) = 0.220 [ 114] Vol = 294.5 Cell: 5.928 5.921 8.389 89.98 90.05 89.91 Volume: 294.47 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.064 MONOCLINIC C-lattice R(int) = 0.272 [ 56] Vol = 294.5 Cell: 8.372 8.389 5.921 89.98 134.93 90.05 Volume: 294.47 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.280 [ 4] Vol = 147.2 Cell: 5.921 5.924 5.928 119.93 90.09 119.92 Volume: 147.23 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 254 0 330 333 495 N (int>3sigma) = 0 0 0 0 254 0 284 289 425 Mean intensity = 0.0 0.0 0.0 0.0 34.2 0.0 82.4 79.1 78.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.3 0.0 26.2 26.2 25.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.204 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 37 112 N I>3s 7 7 27 112 1.0 1.0 0.8 39.9 7.0 7.0 4.0 27.0 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.217 326 Fd-3m 1 1 227 C N N N N 37 2284 0.225 363 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.372260 8.389460 8.384790 90.0186 89.9402 90.0506 ZERR 1.00 0.006827 0.003024 0.000490 0.0036 0.0221 0.0042 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4753636- 631638 125 123 26 4.7 1428600.01 99.55 0.008 0.008 595908- 145697 165 165 26 6.3 257377.03 49.90 0.014 0.016 126628- 64522 135 135 26 5.2 96283.56 20.23 0.026 0.028 44629- 2127 146 145 28 5.2 6075.98 6.15 0.081 0.098 ------------------------------------------------------------------------------------------- 4753636- 2127 571 568 106 5.4 408563.92 42.43 0.011 0.010 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 137 134 26 5.2 707358.11 77.39 0.009 0.008 0.008 1.02-0.78 162 162 26 6.2 446335.89 43.20 0.009 0.010 0.014 0.78-0.66 148 148 26 5.7 299393.88 29.33 0.013 0.014 0.021 0.66-0.59 124 124 28 4.4 166625.92 19.27 0.021 0.022 0.031 ------------------------------------------------------------------------------------------------------ inf-0.59 571 568 106 5.4 408563.92 42.43 0.011 0.010 0.015 inf-0.60 555 552 100 5.5 415856.55 43.18 0.010 0.010 0.015 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 134 27 26 96.3 5.2 707358.11 186.60 0.009 0.004 1.02-0.78 162 26 26 100.0 6.2 446335.89 113.61 0.009 0.006 0.78-0.66 148 26 26 100.0 5.7 299393.88 74.15 0.013 0.009 0.66-0.59 124 31 28 90.3 4.4 166625.92 44.88 0.021 0.016 -------------------------------------------------------------------------------------------- inf-0.59 568 110 106 96.4 5.4 408563.92 105.54 0.011 0.006 inf-0.60 552 101 100 99.0 5.5 415856.55 107.80 0.010 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:30:17 2018) ID: 2932; threads 38; handles 878; mem 517344.00 (1229628.00)kB; time: 1w 4d 22h 35m 48s MEMORY INFO: Memory PF:246.0, Ph:427.0, V:1200.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.2,peak PF: 697.1, WS: 296.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:248.0, Ph:428.0, V:1202.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.0,peak PF: 697.1, WS: 298.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:30:17 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000026 0.000028 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000025 0.000027 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000022 0.000024 0.000013 ) 5.91502 ( 0.00142 ) 5.91640 ( 0.00143 ) 5.92265 ( 0.00105 ) 60.05206 ( 0.02240 ) 89.98756 ( 0.01727 ) 60.01743 ( 0.02524 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:30:17 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000026 0.000028 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000025 0.000027 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000022 0.000024 0.000013 ) M - matrix: 0.021484 -0.014353 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014353 0.028710 -0.014327 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014327 0.021450 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9150(14) 5.9164(14) 5.9227(11) 60.05(2) 89.988(17) 60.02(2) V = 146.73(5) Lattice type P used *** 3D peak analysis started - run 1 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb PROFFITPEAK info: 1609 peaks in the peak location table UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 685 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-14.1 | 44 | 1.130 ( 0.046) | 1.239 ( 0.404) | 1.247 ( 0.628) | 14.2-19.7 | 44 | 1.125 ( 0.067) | 1.150 ( 0.237) | 1.351 ( 0.592) | 19.7-23.6 | 44 | 1.122 ( 0.082) | 1.169 ( 0.370) | 1.291 ( 0.528) | 23.8-28.2 | 44 | 1.102 ( 0.095) | 1.138 ( 0.427) | 1.365 ( 0.471) | 28.4-31.1 | 44 | 1.066 ( 0.091) | 0.983 ( 0.101) | 1.319 ( 0.495) | 31.1-34.5 | 44 | 1.063 ( 0.089) | 0.931 ( 0.110) | 1.305 ( 0.501) | 34.5-37.3 | 44 | 1.033 ( 0.088) | 0.894 ( 0.095) | 1.370 ( 0.566) | 37.4-39.6 | 44 | 1.007 ( 0.113) | 0.898 ( 0.203) | 1.343 ( 0.582) | 39.7-42.7 | 44 | 0.981 ( 0.107) | 0.837 ( 0.088) | 1.184 ( 0.491) | 42.7-49.7 | 46 | 0.998 ( 0.115) | 0.814 ( 0.074) | 1.186 ( 0.515) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.7 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Fitted profile normalization line parameters e1 dimension: a=-0.0031 b=1.12 e2 dimension: a=-0.0107 b=1.29 e3 dimension: a=0.0051 b=0.94 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 4107 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 8009297 lp-corr: 2344269 PROFFITPEAK - Finished at Tue Mar 27 13:30:25 2018 PROFFITMAIN - Started at Tue Mar 27 13:30:25 2018 OTKP changes: 442 1 1 1 Singular = 10, Cryst. Rot. Z Adjusting model LS parameters... OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070135 0.030660 0.088734 ( 0.000026 0.000026 0.000015 ) -0.068211 -0.065964 -0.010738 ( 0.000023 0.000023 0.000013 ) 0.109140 -0.153012 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9213(13) 5.9313(10) 60.04(2) 90.039(16) 59.98(2) V = 147.25(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070135 0.030660 0.088734 ( 0.000026 0.000026 0.000015 ) -0.068211 -0.065964 -0.010738 ( 0.000023 0.000023 0.000013 ) 0.109140 -0.153012 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9297(13) 5.9213(13) 5.9313(10) 60.04(2) 90.039(16) 59.98(2) V = 147.25(4) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070135 0.030660 0.088734 ( 0.000026 0.000026 0.000015 ) -0.068211 -0.065964 -0.010738 ( 0.000023 0.000023 0.000013 ) 0.109140 -0.153012 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9213(13) 5.9313(10) 60.04(2) 90.039(16) 59.98(2) V = 147.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070135 0.030660 0.088734 ( 0.000026 0.000026 0.000015 ) -0.068211 -0.065964 -0.010738 ( 0.000023 0.000023 0.000013 ) 0.109140 -0.153012 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9213(13) 5.9313(10) 60.04(2) 90.039(16) 59.98(2) V = 147.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070135 0.030660 0.088734 ( 0.000026 0.000026 0.000015 ) -0.068211 -0.065964 -0.010738 ( 0.000023 0.000023 0.000013 ) 0.109140 -0.153012 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9213(13) 5.9313(10) 60.04(2) 90.039(16) 59.98(2) V = 147.25(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 26 reflections under beam stop or inside a detector rejection region 4 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof 627 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:30:27 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=273.0000 max=12222183.0000 PROFFIT INFO: signal sum lp corr: min=632.0289 max=2944647.7864 PROFFIT INFO: background sum: min=1296.0000 max=6854.0000 PROFFIT INFO: background sum sig2: min=682.0000 max=6416.0000 PROFFIT INFO: num of signal pixels: min=63 max=526 PROFFIT INFO: Inet: min=1011.2463 max=4711436.5000 PROFFIT INFO: sig(Inet): min=183.4776 max=47365.1211 PROFFIT INFO: Inet/sig(Inet): min=1.08 max=228.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 22 60 133 147 243 408 565 627 Percent 0.0 0.0 0.6 3.5 9.6 21.2 23.4 38.8 65.1 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 627 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 627 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711437- 1270687 62 2090679.34 132.03 100.00 1265370- 756471 62 975868.71 109.11 100.00 746798- 315422 62 481139.14 99.46 100.00 315122- 183793 62 228074.05 71.73 100.00 183546- 147036 62 167455.57 55.30 100.00 146810- 104808 62 121607.93 36.97 100.00 104433- 81076 62 91607.86 30.42 100.00 80697- 5881 62 45139.15 20.39 100.00 5836- 3440 62 4470.00 5.72 96.77 3438- 1011 69 2667.61 4.13 71.01 ------------------------------------------------------------------------------------ 4711437- 1011 627 416202.00 55.94 96.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 62 833029.84 84.31 100.00 1.28- 1.08 62 639991.04 72.26 96.77 1.05- 0.96 62 421955.20 62.36 98.39 0.93- 0.85 62 504382.77 63.80 98.39 0.83- 0.76 62 410538.24 62.83 96.77 0.75- 0.70 62 315646.61 50.93 98.39 0.70- 0.65 62 314355.64 49.26 98.39 0.65- 0.60 62 307851.08 44.84 91.94 0.60- 0.55 62 218942.14 36.84 93.55 0.55- 0.42 69 217734.98 34.41 92.75 ------------------------------------------------------------------------------------ 5.27- 0.42 627 416202.00 55.94 96.49 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:30:27 2018 Sorting 627 observations 143 unique observations with > 7.00 F2/sig(F2) 627 observations in 1 runs Run # start # end # total # 1 0 108 109 Total number of frames 109 Maximum number of 143 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 627 observations in 1 runs Run # start # end # total # 1 0 108 109 Total number of frames 109 498 observations > 7.00 F2/sig(F2) 498 observations in 1 runs Run # start # end # total # 1 0 108 109 Total number of frames 109 Frame #58 of 109 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.2 (Out of 498 removed 89 = 409, unique = 128) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 409 observations in 1 runs Run # start # end # total # 1 0 108 109 Total number of frames 109 Frame #14 of 109 skipped from refinement Frame #58 of 109 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 128 unique data precomputed (should be 128) 128 unique data with 409 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.2 (Out of 409 removed 0 = 409, unique = 128) 128 unique data precomputed (should be 128) 128 unique data with 409 observations RMS deviation of equivalent data = 0.63946 Rint = 0.54815 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.51722, wR= 3.65529 Trying model 1 (ne=2, no=0)... Results: Rint= 0.91794, wR= 1.74842, Acormin=-0.248, Acormax=1.258, Acor_av=0.168 F test: Probability=0.000, F= 0.312 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88773, wR= 3.06385, Acormin=-0.450, Acormax=0.818, Acor_av=0.048 F test: Probability=0.000, F= 0.330 Trying model 3 (ne=4, no=0)... Results: Rint= 0.93266, wR= 1.78749, Acormin=-0.199, Acormax=0.838, Acor_av=0.026 F test: Probability=0.000, F= 0.292 Trying model 4 (ne=4, no=1)... Results: Rint= 0.95715, wR= 2.29898, Acormin=-0.279, Acormax=0.664, Acor_av=0.006 F test: Probability=0.000, F= 0.274 Trying model 5 (ne=4, no=3)... Results: Rint= 0.94323, wR= 2.21236, Acormin=-0.141, Acormax=0.244, Acor_av=-0.001 F test: Probability=0.000, F= 0.275 Trying model 6 (ne=6, no=0)... Results: Rint= 0.88066, wR= 1.69684, Acormin=-0.086, Acormax=0.642, Acor_av=0.001 F test: Probability=0.000, F= 0.311 Trying model 7 (ne=6, no=1)... Results: Rint= 0.90023, wR= 1.91181, Acormin=-0.092, Acormax=0.636, Acor_av=0.000 F test: Probability=0.000, F= 0.294 Trying model 8 (ne=6, no=3)... Results: Rint= 0.84713, wR= 1.62591, Acormin=-0.149, Acormax=0.390, Acor_av=0.001 F test: Probability=0.000, F= 0.323 Trying model 9 (ne=6, no=5)... Results: Rint= 0.80817, wR= 1.91109, Acormin=-0.042, Acormax=0.102, Acor_av=0.002 F test: Probability=0.000, F= 0.339 Trying model 10 (ne=8, no=0)... Results: Rint= 0.93486, wR= 1.72713, Acormin=-0.108, Acormax=0.392, Acor_av=-0.001 F test: Probability=0.000, F= 0.258 Trying model 11 (ne=8, no=1)... Results: Rint= 0.93455, wR= 1.56130, Acormin=-0.099, Acormax=0.386, Acor_av=-0.001 F test: Probability=0.000, F= 0.255 Trying model 12 (ne=8, no=3)... Results: Rint= 0.72111, wR= 1.50739, Acormin=-0.020, Acormax=0.010, Acor_av=0.001 F test: Probability=0.000, F= 0.415 Trying model 13 (ne=8, no=5)... Results: Rint= 0.66067, wR= 1.53343, Acormin=-0.019, Acormax=0.052, Acor_av=0.001 F test: Probability=0.000, F= 0.470 Trying model 14 (ne=8, no=7)... Results: Rint= 0.43350, wR= 1.25728, Acormin=-0.016, Acormax=0.091, Acor_av=0.003 F test: Probability=0.539, F= 1.014 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.70671 There are 107 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 111 pars with 6216 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.63946 Using Levenberg-Marquardt: 0.00010 New wR= 0.59932 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.54815 with corrections 0.49980 Rint for all data: 0.70671 with corrections 0.67540 2 observations identified as outliers and rejected Cycle 2 wR= 0.58914 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.57012 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.52549 with corrections 0.49670 Rint for all data: 0.70671 with corrections 0.68388 1 observations identified as outliers and rejected Cycle 3 wR= 0.56724 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.57071 Using Levenberg-Marquardt: 0.10000 New wR= 0.55383 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51722 with corrections 0.51189 Rint for all data: 0.70671 with corrections 0.70217 1 observations identified as outliers and rejected Cycle 4 wR= 0.54757 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.54110 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.51556 with corrections 0.53432 Rint for all data: 0.70671 with corrections 0.71926 1 observations identified as outliers and rejected Cycle 5 wR= 0.53794 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.52816 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.50867 with corrections 0.56496 Rint for all data: 0.70671 with corrections 0.74115 0 observations identified as outliers and rejected Final wR= 0.52816 Final frame scales: Min= 0.7364 Max= 7.1611 Final absorption correction factors: Amin= 0.0206 Amax= 4.3625 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 107 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 111 pars with 6216 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.87041 Using Levenberg-Marquardt: 0.00010 New wR= 0.64664 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.50867 with corrections 1.22969 Rint for all data: 0.70671 with corrections 1.27529 1 observations identified as outliers and rejected Cycle 2 wR= 0.63624 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 New wR= 0.63588 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.50739 with corrections 1.22748 Rint for all data: 0.70671 with corrections 1.27317 Final wR= 0.63588 Frame scales out of range! Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 93 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 92 pars with 4278 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.29866 Using Levenberg-Marquardt: 0.00010 New wR= 0.61473 There are 4 clusters with unrefined scales (size 1-9) Rint for refined data: 0.50739 with corrections 0.60054 Rint for all data: 0.70671 with corrections 0.77344 0 observations identified as outliers and rejected Cycle 2 wR= 0.61653 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57570 There are 4 clusters with unrefined scales (size 1-9) Rint for refined data: 0.50739 with corrections 0.59724 Rint for all data: 0.70671 with corrections 0.76841 0 observations identified as outliers and rejected Cycle 3 wR= 0.58356 Using Levenberg-Marquardt: 0.01000 New wR= 0.56624 There are 4 clusters with unrefined scales (size 1-9) Rint for refined data: 0.50739 with corrections 0.62352 Rint for all data: 0.70671 with corrections 0.79124 0 observations identified as outliers and rejected Cycle 4 wR= 0.58961 Using Levenberg-Marquardt: 0.00100 New wR= 0.57133 There are 4 clusters with unrefined scales (size 1-9) Rint for refined data: 0.50739 with corrections 0.69986 Rint for all data: 0.70671 with corrections 0.86387 0 observations identified as outliers and rejected Cycle 5 wR= 0.60325 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.62242 Using Levenberg-Marquardt: 1.00000 New wR= 0.59188 There are 4 clusters with unrefined scales (size 1-9) Rint for refined data: 0.50739 with corrections 0.69740 Rint for all data: 0.70671 with corrections 0.85992 0 observations identified as outliers and rejected Final wR= 0.59188 Final frame scales: Min= 1.0000 Max= 68.4434 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 2 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 1 pars with 1 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.95841 Using Levenberg-Marquardt: 0.00010 New wR= 0.61024 There are 2 clusters with unrefined scales (size 38-70) Rint for refined data: 0.50739 with corrections 0.50739 Rint for all data: 0.70671 with corrections 0.70671 0 observations identified as outliers and rejected Cycle 2 wR= 0.60872 Using Levenberg-Marquardt: 0.00001 New wR= 0.60861 There are 2 clusters with unrefined scales (size 38-70) Rint for refined data: 0.50739 with corrections 0.50739 Rint for all data: 0.70671 with corrections 0.70671 Final wR= 0.60861 Final frame scales: Min= 9.7347 Max= 9.7347 Frame scales outside specified range! Trying one more time after skipping bad frame scales SCALE3 WARNING: No scale needs refinement Frame scaling turned off SCALE3 ERROR: No parameters to be refined! ! SCALE3 WARNING: Frame scaling turned off due to lack of scales requiring refinement Can't fit requested scale/empirical absorption model (pTmpToScale3AbspackHKL) ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/1 frame:1/109 627 reflections read from tmp file 504 reflections are rejected (390 as outliers, 114 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 39 11 3 Initial Chi^2= 0.59093 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.89248 Current error model SIG(F2)^2 = 168.06*I_RAW + 0.00*I_BACK+(0.03585*)^2 Cycle 2, Chi^2= 0.99852 Current error model SIG(F2)^2 = 172.01*I_RAW + 0.00*I_BACK+(0.02704*)^2 Cycle 3, Chi^2= 1.00020 Current error model SIG(F2)^2 = 177.92*I_RAW + 0.00*I_BACK+(0.02512*)^2 Cycle 4, Chi^2= 1.00003 Current error model SIG(F2)^2 = 178.64*I_RAW + 0.00*I_BACK+(0.02491*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 178.68*I_RAW + 0.00*I_BACK+(0.02490*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 178.68*I_RAW + 0.00*I_BACK+(0.02490*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711437- 1270687 62 2090679.34 91.97 100.00 1265370- 756471 62 975868.71 46.73 100.00 746798- 315422 62 481139.14 40.43 100.00 315122- 183793 62 228074.05 30.54 100.00 183546- 147036 62 167455.57 23.12 100.00 146810- 104808 62 121607.93 16.78 100.00 104433- 81076 62 91607.86 14.23 100.00 80697- 5881 62 45139.15 10.09 100.00 5836- 3440 62 4470.00 3.91 83.87 3438- 1011 69 2667.61 3.17 53.62 ------------------------------------------------------------------------------------ 4711437- 1011 627 416202.00 27.82 93.30 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 62 833029.84 47.95 98.39 1.28- 1.08 62 639991.04 45.19 95.16 1.05- 0.96 62 421955.20 31.83 96.77 0.93- 0.85 62 504382.77 32.12 91.94 0.83- 0.76 62 410538.24 24.37 95.16 0.75- 0.70 62 315646.61 24.23 96.77 0.70- 0.65 62 314355.64 22.45 91.94 0.65- 0.60 62 307851.08 19.29 87.10 0.60- 0.55 62 218942.14 16.91 88.71 0.55- 0.42 69 217734.98 15.28 91.30 ------------------------------------------------------------------------------------ 5.27- 0.42 627 416202.00 27.82 93.30 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 62 833029.84 47.95 98.39 5.27- 1.08 124 736510.44 46.57 96.77 5.27- 0.96 186 631658.69 41.65 96.77 5.27- 0.85 248 599839.71 39.27 95.56 5.27- 0.76 310 561979.42 36.29 95.48 5.27- 0.70 372 520923.95 34.28 95.70 5.27- 0.65 434 491414.19 32.59 95.16 5.27- 0.60 496 468468.80 30.93 94.15 5.27- 0.55 558 440743.62 29.37 93.55 5.27- 0.42 627 416202.00 27.82 93.30 ------------------------------------------------------------------------------------ 5.27- 0.42 627 416202.00 27.82 93.30 Scale applied to data: s=0.212249 (maximum obs:4711436.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.707; Rsigma 0.024: data 627 -> merged 244 With outlier rejection... Rint 0.507; Rsigma 0.025: data 530 -> merged 244 Rejected total: 97, method kkm 95, method Blessing 2 Completeness direct cell (a, b, c) = (5.281, 5.281, 5.281), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.425520, 5.280569 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.46 15 15 2.40 100.00 36 1.46 - 1.13 15 15 4.47 100.00 67 1.08 - 0.96 15 15 3.60 100.00 54 0.96 - 0.86 15 15 3.13 100.00 47 0.86 - 0.79 15 15 2.80 100.00 42 0.79 - 0.73 15 15 2.47 100.00 37 0.73 - 0.69 15 15 2.13 100.00 32 0.69 - 0.65 15 15 1.93 100.00 29 0.65 - 0.64 15 15 1.73 100.00 26 0.63 - 0.60 21 21 1.62 100.00 34 --------------------------------------------------------------- 5.93 - 0.60 156 156 2.59 100.00 404 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:30:27 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929678 5.921257 5.931321 60.0379 90.0393 59.9789 530 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 255 277 262 269 397 357 358 530 N (int>3sigma) = 0 240 277 247 257 382 334 336 496 Mean intensity = 0.0 69.3 36.0 68.6 76.3 57.4 83.7 78.0 79.1 Mean int/sigma = 0.0 25.2 22.9 25.2 26.3 24.4 26.1 25.4 25.4 Lattice type: P chosen Volume: 147.25 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.921 5.924 5.928 119.94 90.07 119.92 Niggli form: a.a = 35.061 b.b = 35.089 c.c = 35.141 b.c = -17.524 a.c = -0.046 a.b = -17.495 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.107 CUBIC F-lattice R(int) = 0.059 [ 379] Vol = 589.0 Cell: 8.373 8.390 8.384 90.02 89.94 90.06 Volume: 588.98 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.056 [ 253] Vol = 441.7 Cell: 5.924 5.921 14.531 89.96 90.07 119.92 Volume: 441.74 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 68] Vol = 441.7 Trigonal Cell: 5.924 5.921 14.531 89.96 90.07 119.92 Volume: 441.74 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.055 [ 216] Vol = 294.5 Cell: 5.930 5.931 8.373 89.91 90.00 90.04 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.107 TETRAGONAL I-lattice R(int) = 0.055 [ 216] Vol = 294.5 Cell: 5.930 5.931 8.373 89.91 90.00 90.04 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.091 ORTHORHOMBIC I-lattice R(int) = 0.039 [ 265] Vol = 294.5 Cell: 5.930 8.373 5.931 89.91 89.96 90.00 Volume: 294.49 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.029 MONOCLINIC I-lattice R(int) = 0.037 [ 156] Vol = 294.5 Cell: 8.373 5.930 5.931 90.04 90.09 90.00 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.058 MONOCLINIC I-lattice R(int) = 0.045 [ 141] Vol = 294.5 Cell: 5.928 5.921 8.390 89.97 90.05 89.93 Volume: 294.49 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.075 MONOCLINIC C-lattice R(int) = 0.067 [ 64] Vol = 294.5 Cell: 8.373 8.390 5.921 89.97 134.93 90.06 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.070 [ 6] Vol = 147.2 Cell: 5.921 5.924 5.928 119.94 90.07 119.92 Volume: 147.25 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 277 0 357 353 530 N (int>3sigma) = 0 0 0 0 277 0 334 335 496 Mean intensity = 0.0 0.0 0.0 0.0 36.0 0.0 83.7 79.7 79.1 Mean int/sigma = 0.0 0.0 0.0 0.0 22.9 0.0 26.1 24.7 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.150 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 39 119 N I>3s 7 7 35 119 1.0 1.0 0.9 42.0 8.2 8.2 4.6 26.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.059 359 Fd-3m 1 1 227 C N N N N 37 2284 0.061 396 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.373183 8.389869 8.384116 90.0159 89.9353 90.0590 ZERR 1.00 0.006259 0.002834 0.000447 0.0028 0.0205 0.0031 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4310025- 895869 79 69 27 2.6 1360456.52 53.92 0.427 0.329 886487- 602715 70 59 27 2.2 725753.60 40.51 0.748 0.674 588010- 392501 98 70 27 2.6 263648.56 22.86 0.678 0.707 386223- 255771 87 73 27 2.7 245000.10 25.23 0.473 0.537 246827- 137270 82 69 27 2.6 152344.04 22.23 0.285 0.216 136682- 99671 66 58 27 2.1 124606.23 18.90 0.374 0.324 97725- 81076 47 40 27 1.5 93819.12 14.54 0.158 0.158 80489- 8732 61 55 27 2.0 53065.66 10.52 0.385 0.296 6307- 1350 37 37 28 1.3 3721.74 3.55 0.138 0.138 ------------------------------------------------------------------------------------------- 4310025- 1350 627 530 244 2.2 372791.23 25.42 0.507 0.448 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.18 94 82 27 3.0 681023.97 43.49 0.433 0.341 0.017 1.15-0.89 130 104 27 3.9 399663.21 29.56 0.612 0.591 0.020 0.88-0.75 97 78 28 2.8 378833.20 23.18 0.492 0.381 0.029 0.75-0.68 80 61 28 2.2 402162.47 26.99 0.473 0.423 0.024 0.68-0.63 60 49 27 1.8 191227.53 16.70 0.441 0.435 0.041 0.62-0.59 51 45 27 1.7 315181.54 19.36 0.452 0.455 0.033 0.58-0.55 44 41 28 1.5 157874.16 14.59 0.746 0.746 0.043 0.55-0.51 40 39 28 1.4 252562.49 16.18 0.505 0.505 0.039 0.51-0.43 31 31 24 1.3 200432.72 14.87 0.823 0.823 0.042 ------------------------------------------------------------------------------------------------------ inf-0.43 627 530 244 2.2 372791.23 25.42 0.507 0.448 0.025 inf-0.60 494 404 156 2.6 422468.44 28.43 0.500 0.429 0.023 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.18 82 27 27 100.0 3.0 681023.97 102.32 0.433 0.012 1.15-0.89 104 27 27 100.0 3.9 399663.21 73.36 0.612 0.013 0.88-0.75 78 28 28 100.0 2.8 378833.20 48.46 0.492 0.019 0.75-0.68 61 28 28 100.0 2.2 402162.47 47.49 0.473 0.017 0.68-0.63 49 27 27 100.0 1.8 191227.53 24.62 0.441 0.030 0.62-0.59 45 28 27 96.4 1.7 315181.54 28.47 0.452 0.023 0.58-0.55 41 33 28 84.8 1.5 157874.16 21.25 0.746 0.031 0.55-0.51 39 43 28 65.1 1.4 252562.49 21.41 0.505 0.029 0.51-0.43 31 163 24 14.7 1.3 200432.72 20.09 0.823 0.030 -------------------------------------------------------------------------------------------- inf-0.43 530 404 244 60.4 2.2 372791.23 51.91 0.507 0.018 inf-0.60 404 156 156 100.0 2.6 422468.44 61.32 0.500 0.016 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 -2.0 1.0 1.0 0.0 -1.0 1.0 0.0 1.0 No constraint UB - matrix: -0.015330 -0.079435 0.024629 ( 0.000013 0.000011 0.000013 ) 0.032982 -0.028737 -0.072456 ( 0.000011 0.000010 0.000012 ) 0.076506 -0.003432 0.036065 ( 0.000011 0.000010 0.000012 ) M - matrix: 0.007176 0.000007 -0.000008 ( 0.000002 0.000001 0.000001 ) 0.000007 0.007147 0.000002 ( 0.000001 0.000002 0.000001 ) -0.000008 0.000002 0.007157 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.015330 -0.079435 0.024629 ( 0.000013 0.000011 0.000013 ) 0.032982 -0.028737 -0.072456 ( 0.000011 0.000010 0.000012 ) 0.076506 -0.003432 0.036065 ( 0.000011 0.000010 0.000012 ) M - matrix: 0.007154 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007154 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007154 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3732(11) 8.3899(12) 8.3841(12) 90.016(11) 89.935(11) 90.059(11) V = 588.98(14) unit cell: 8.3824(4) 8.3824(4) 8.3824(4) 90.0 90.0 90.0 V = 588.98(5) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=273.0000 max=12222183.0000 PROFFIT INFO: signal sum lp corr: min=632.0289 max=2944647.7864 PROFFIT INFO: background sum: min=1296.0000 max=6854.0000 PROFFIT INFO: background sum sig2: min=682.0000 max=6416.0000 PROFFIT INFO: num of signal pixels: min=63 max=526 PROFFIT INFO: Inet: min=1011.2463 max=4711436.5000 PROFFIT INFO: sig(Inet): min=183.4776 max=47365.1211 PROFFIT INFO: Inet/sig(Inet): min=1.08 max=228.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 44 120 266 294 486 816 1130 1254 Percent 0.0 0.0 0.6 3.5 9.6 21.2 23.4 38.8 65.1 90.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 627 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 627 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711437- 1270687 62 2090679.34 132.03 100.00 1265370- 756471 62 975868.71 109.11 100.00 746798- 315422 62 481139.14 99.46 100.00 315122- 183793 62 228074.05 71.73 100.00 183546- 147036 62 167455.57 55.30 100.00 146810- 104808 62 121607.93 36.97 100.00 104433- 81076 62 91607.86 30.42 100.00 80697- 5881 62 45139.15 20.39 100.00 5836- 3440 62 4470.00 5.72 96.77 3438- 1011 69 2667.61 4.13 71.01 ------------------------------------------------------------------------------------ 4711437- 1011 627 416202.00 55.94 96.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 62 790151.96 87.54 100.00 1.39- 1.09 62 863471.96 77.44 100.00 1.09- 0.96 62 412759.52 70.86 100.00 0.96- 0.85 62 478214.17 69.80 96.77 0.85- 0.80 62 454837.97 67.48 100.00 0.80- 0.73 62 266021.88 42.65 100.00 0.73- 0.70 62 239120.88 37.95 85.48 0.70- 0.65 62 349268.80 51.34 98.39 0.65- 0.63 62 169027.86 28.65 88.71 0.63- 0.59 69 167252.20 28.77 95.65 ------------------------------------------------------------------------------------ 4.83- 0.59 627 416202.00 55.94 96.49 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:30:28 2018 Sorting 627 observations 76 unique observations with > 7.00 F2/sig(F2) 627 observations in 1 runs Run # start # end # total # 1 0 108 109 Total number of frames 109 Maximum number of 76 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 627 observations in 1 runs Run # start # end # total # 1 0 54 55 Total number of frames 55 498 observations > 7.00 F2/sig(F2) 498 observations in 1 runs Run # start # end # total # 1 0 54 55 Total number of frames 55 Removing 'redundancy=1' reflections Average redundancy: 6.3 (Out of 498 removed 9 = 489, unique = 78) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 489 observations in 1 runs Run # start # end # total # 1 0 54 55 Total number of frames 55 78 unique data precomputed (should be 78) 78 unique data with 489 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.3 (Out of 489 removed 0 = 489, unique = 78) 78 unique data precomputed (should be 78) 78 unique data with 489 observations RMS deviation of equivalent data = 0.07517 Rint = 0.06416 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.06050, wR= 0.07750 Trying model 1 (ne=2, no=0)... Results: Rint= 0.03149, wR= 0.04159, Acormin=0.801, Acormax=1.123, Acor_av=0.893 F test: Probability=1.000, F= 3.647 Trying model 2 (ne=2, no=1)... Results: Rint= 0.02607, wR= 0.03376, Acormin=0.815, Acormax=1.203, Acor_av=0.916 F test: Probability=1.000, F= 1.448 Trying model 3 (ne=4, no=0)... Results: Rint= 0.02137, wR= 0.02810, Acormin=0.801, Acormax=1.279, Acor_av=0.961 F test: Probability=1.000, F= 1.466 Trying model 4 (ne=4, no=1)... Results: Rint= 0.01852, wR= 0.02425, Acormin=0.839, Acormax=1.316, Acor_av=0.974 F test: Probability=0.997, F= 1.321 Trying model 5 (ne=4, no=3)... Results: Rint= 0.01694, wR= 0.02193, Acormin=0.838, Acormax=1.311, Acor_av=0.977 F test: Probability=0.944, F= 1.175 Trying model 6 (ne=6, no=0)... Results: Rint= 0.01809, wR= 0.02371, Acormin=0.827, Acormax=1.301, Acor_av=0.974 F test: Probability=0.582, F= 1.021 Trying model 7 (ne=6, no=1)... Results: Rint= 0.01618, wR= 0.02065, Acormin=0.846, Acormax=1.347, Acor_av=0.977 F test: Probability=0.990, F= 1.266 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01555, wR= 0.01923, Acormin=0.842, Acormax=1.305, Acor_av=0.979 F test: Probability=0.723, F= 1.063 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01454, wR= 0.01821, Acormin=0.846, Acormax=1.326, Acor_av=0.981 F test: Probability=0.944, F= 1.180 Final absorption model (ne=6, no=1): Rint= 0.01618, Acormin=0.846, Acormax=1.347, Acor_av=0.977 Combined refinement in use Rint: 0.06431 There are 55 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 1 (30 parameters) Refinement control: 84 pars with 3570 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.07517 Using Levenberg-Marquardt: 0.00010 New wR= 0.01742 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06416 with corrections 0.01433 Rint for all data: 0.06431 with corrections 0.01458 0 observations identified as outliers and rejected Cycle 2 wR= 0.01742 Using Levenberg-Marquardt: 0.00001 New wR= 0.01715 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06416 with corrections 0.01420 Rint for all data: 0.06431 with corrections 0.01445 0 observations identified as outliers and rejected Cycle 3 wR= 0.01715 Using Levenberg-Marquardt: 0.00000 New wR= 0.01717 Using Levenberg-Marquardt: 0.00001 New wR= 0.01717 Using Levenberg-Marquardt: 0.00010 New wR= 0.01717 Using Levenberg-Marquardt: 0.00100 New wR= 0.01717 Using Levenberg-Marquardt: 0.01000 New wR= 0.01717 Using Levenberg-Marquardt: 0.10000 New wR= 0.01715 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.06416 with corrections 0.01424 Rint for all data: 0.06431 with corrections 0.01448 Final wR= 0.01715 Final frame scales: Min= 0.9482 Max= 1.0083 Final absorption correction factors: Amin= 0.7039 Amax= 1.1332 PROFFIT INFO: Inet (after scale3 abspack): min=952.9166 max=4726631.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=189.4011 max=46438.0625 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/1 frame:1/109 627 reflections read from tmp file 18 reflections are rejected (10 as outliers, 8 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 13 5 12 15 15 8 7 6 17 Initial Chi^2= 0.27122 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.11110 Current error model SIG(F2)^2 = 110.60*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 122.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 122.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4726631- 1262483 62 2094567.73 137.73 100.00 1226659- 737144 62 956457.63 64.53 100.00 733125- 317950 62 485296.29 67.50 100.00 317086- 185995 62 227167.60 44.22 100.00 184783- 149835 62 166501.66 31.80 100.00 147560- 104835 62 117888.84 22.27 100.00 103887- 80918 62 93113.87 18.69 100.00 80536- 6064 62 45724.51 13.36 100.00 6045- 3365 62 4473.83 4.89 100.00 3359- 953 69 2649.33 4.12 91.30 ------------------------------------------------------------------------------------ 4726631- 953 627 414731.59 40.50 99.04 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 62 793957.03 91.21 100.00 1.39- 1.09 62 870960.52 74.41 100.00 1.09- 0.96 62 417948.41 43.95 100.00 0.96- 0.85 62 466833.82 41.85 98.39 0.85- 0.80 62 450964.13 40.38 100.00 0.80- 0.73 62 262528.97 26.02 100.00 0.73- 0.70 62 236288.39 23.27 95.16 0.70- 0.65 62 342229.35 30.78 100.00 0.65- 0.63 62 166676.55 17.84 96.77 0.63- 0.59 69 166908.70 17.86 100.00 ------------------------------------------------------------------------------------ 4.83- 0.59 627 414731.59 40.50 99.04 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 62 793957.03 91.21 100.00 4.83- 1.09 124 832458.78 82.81 100.00 4.83- 0.96 186 694288.65 69.86 100.00 4.83- 0.85 248 637424.94 62.86 99.60 4.83- 0.80 310 600132.78 58.36 99.68 4.83- 0.73 372 543865.48 52.97 99.73 4.83- 0.70 434 499925.90 48.73 99.08 4.83- 0.65 496 480213.83 46.48 99.19 4.83- 0.63 558 445376.35 43.30 98.92 4.83- 0.59 627 414731.59 40.50 99.04 ------------------------------------------------------------------------------------ 4.83- 0.59 627 414731.59 40.50 99.04 Scale applied to data: s=0.211567 (maximum obs:4726631.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.016: data 627 -> merged 106 With outlier rejection... Rint 0.013; Rsigma 0.016: data 623 -> merged 106 Rejected total: 4, method kkm 4, method Blessing 0 Completeness direct cell (a, b, c) = (8.382, 8.382, 8.382), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586884, 4.839569 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.71 9 10 3.56 90.00 32 1.61 - 1.21 10 10 5.40 100.00 54 1.17 - 1.02 10 10 7.30 100.00 73 0.99 - 0.89 10 10 7.20 100.00 72 0.88 - 0.81 10 10 7.10 100.00 71 0.81 - 0.74 10 10 5.90 100.00 59 0.73 - 0.71 10 10 6.90 100.00 69 0.70 - 0.66 10 10 5.90 100.00 59 0.66 - 0.64 10 10 5.10 100.00 51 0.63 - 0.60 12 12 5.58 100.00 67 --------------------------------------------------------------- 5.93 - 0.60 101 102 6.01 99.02 607 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:30:27 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.929678 5.921257 5.931321 60.0379 90.0393 59.9789 530 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 255 277 262 269 397 357 358 530 N (int>3sigma) = 0 240 277 247 257 382 334 336 496 Mean intensity = 0.0 69.3 36.0 68.6 76.3 57.4 83.7 78.0 79.1 Mean int/sigma = 0.0 25.2 22.9 25.2 26.3 24.4 26.1 25.4 25.4 Lattice type: P chosen Volume: 147.25 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Unitcell: 5.921 5.924 5.928 119.94 90.07 119.92 Niggli form: a.a = 35.061 b.b = 35.089 c.c = 35.141 b.c = -17.524 a.c = -0.046 a.b = -17.495 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.107 CUBIC F-lattice R(int) = 0.059 [ 379] Vol = 589.0 Cell: 8.373 8.390 8.384 90.02 89.94 90.06 Volume: 588.98 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.056 [ 253] Vol = 441.7 Cell: 5.924 5.921 14.531 89.96 90.07 119.92 Volume: 441.74 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.094 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 68] Vol = 441.7 Trigonal Cell: 5.924 5.921 14.531 89.96 90.07 119.92 Volume: 441.74 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 0.0000 1.0000 -2.0000 3.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.136 TETRAGONAL I-lattice R(int) = 0.055 [ 216] Vol = 294.5 Cell: 5.930 5.931 8.373 89.91 90.00 90.04 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.107 TETRAGONAL I-lattice R(int) = 0.055 [ 216] Vol = 294.5 Cell: 5.930 5.931 8.373 89.91 90.00 90.04 Volume: 294.49 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.091 ORTHORHOMBIC I-lattice R(int) = 0.039 [ 265] Vol = 294.5 Cell: 5.930 8.373 5.931 89.91 89.96 90.00 Volume: 294.49 Matrix:-1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.029 MONOCLINIC I-lattice R(int) = 0.037 [ 156] Vol = 294.5 Cell: 8.373 5.930 5.931 90.04 90.09 90.00 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.058 MONOCLINIC I-lattice R(int) = 0.045 [ 141] Vol = 294.5 Cell: 5.928 5.921 8.390 89.97 90.05 89.93 Volume: 294.49 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.075 MONOCLINIC C-lattice R(int) = 0.067 [ 64] Vol = 294.5 Cell: 8.373 8.390 5.921 89.97 134.93 90.06 Volume: 294.49 Matrix: 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.070 [ 6] Vol = 147.2 Cell: 5.921 5.924 5.928 119.94 90.07 119.92 Volume: 147.25 Matrix: 0.0000 1.0000 0.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 277 0 357 353 530 N (int>3sigma) = 0 0 0 0 277 0 334 335 496 Mean intensity = 0.0 0.0 0.0 0.0 36.0 0.0 83.7 79.7 79.1 Mean int/sigma = 0.0 0.0 0.0 0.0 22.9 0.0 26.1 24.7 25.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.150 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 7 7 39 119 N I>3s 7 7 35 119 1.0 1.0 0.9 42.0 8.2 8.2 4.6 26.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.059 359 Fd-3m 1 1 227 C N N N N 37 2284 0.061 396 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.373183 8.389869 8.384116 90.0159 89.9353 90.0590 ZERR 1.00 0.006259 0.002834 0.000447 0.0028 0.0205 0.0031 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4692904- 625769 137 135 26 5.2 1424383.49 94.27 0.010 0.010 596990- 142999 180 179 26 6.9 256546.83 46.66 0.016 0.017 125991- 64680 151 151 26 5.8 95574.88 18.79 0.028 0.031 43847- 2315 159 158 28 5.6 5912.90 5.67 0.089 0.107 ------------------------------------------------------------------------------------------- 4692904- 2315 627 623 106 5.9 407030.02 39.82 0.013 0.013 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 149 145 26 5.6 726981.67 74.57 0.010 0.009 0.009 1.02-0.78 177 177 26 6.8 428304.41 39.52 0.011 0.013 0.016 0.78-0.66 165 165 26 6.3 303106.16 27.76 0.015 0.017 0.023 0.66-0.59 136 136 28 4.9 164301.19 17.81 0.025 0.028 0.034 ------------------------------------------------------------------------------------------------------ inf-0.59 627 623 106 5.9 407030.02 39.82 0.013 0.013 0.016 inf-0.60 609 605 100 6.0 414066.05 40.53 0.013 0.013 0.016 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 145 27 26 96.3 5.6 726981.67 188.48 0.010 0.004 1.02-0.78 177 26 26 100.0 6.8 428304.41 108.11 0.011 0.006 0.78-0.66 165 26 26 100.0 6.3 303106.16 73.80 0.015 0.010 0.66-0.59 136 31 28 90.3 4.9 164301.19 43.16 0.025 0.017 -------------------------------------------------------------------------------------------- inf-0.59 623 110 106 96.4 5.9 407030.02 103.55 0.013 0.006 inf-0.60 605 101 100 99.0 6.0 414066.05 105.75 0.013 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:37:32 2018) ID: 2932; threads 39; handles 878; mem 517324.00 (1237820.00)kB; time: 1w 4d 22h 43m 2s MEMORY INFO: Memory PF:254.0, Ph:431.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.2,peak PF: 697.1, WS: 296.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:257.0, Ph:431.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.0,peak PF: 697.1, WS: 298.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:37:32 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000026 0.000026 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000023 0.000023 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000023 0.000013 ) 5.91502 ( 0.00130 ) 5.91640 ( 0.00130 ) 5.92265 ( 0.00101 ) 60.05206 ( 0.02102 ) 89.98756 ( 0.01627 ) 60.01743 ( 0.02300 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 31 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 aP Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:37:32 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000026 0.000026 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000023 0.000023 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014351 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9150(13) 5.9164(13) 5.9227(10) 60.05(2) 89.988(16) 60.02(2) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.083 ( 0.108) | 1.073 ( 0.135) | 1.145 ( 0.399) | 0.84- 0.81 | 44 | 1.105 ( 0.099) | 1.023 ( 0.124) | 1.367 ( 0.511) | 0.81- 0.73 | 44 | 1.095 ( 0.086) | 0.996 ( 0.125) | 1.322 ( 0.491) | 0.73- 0.69 | 44 | 1.089 ( 0.080) | 0.930 ( 0.110) | 1.402 ( 0.496) | 0.69- 0.66 | 44 | 1.076 ( 0.070) | 0.883 ( 0.089) | 1.376 ( 0.477) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.061 ( 0.109) | 0.998 ( 0.252) | 1.316 ( 0.892) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088658 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010700 ( 0.000027 0.000027 0.000015 ) 0.109063 -0.152749 0.115660 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028586 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9265(15) 5.9308(15) 5.9444(11) 60.01(2) 90.018(18) 60.02(3) V = 147.79(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070137 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068210 -0.065969 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109138 -0.153002 0.116014 ( 0.000024 0.000023 0.000013 ) M - matrix: 0.021483 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028702 -0.014322 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014322 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9313(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070137 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068210 -0.065969 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109138 -0.153002 0.116014 ( 0.000024 0.000023 0.000013 ) M - matrix: 0.021483 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028702 -0.014322 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014322 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9313(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.707) | 1.567 ( 2.300) | 1.32- 1.09 | 44 | 1.063 ( 0.112) | 1.086 ( 0.140) | 1.140 ( 0.482) | 1.09- 0.96 | 44 | 1.060 ( 0.106) | 1.078 ( 0.148) | 1.126 ( 0.473) | 0.94- 0.84 | 44 | 1.078 ( 0.105) | 1.066 ( 0.134) | 1.141 ( 0.405) | 0.84- 0.81 | 44 | 1.110 ( 0.099) | 1.023 ( 0.124) | 1.355 ( 0.482) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.990 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.092 ( 0.076) | 0.948 ( 0.113) | 1.397 ( 0.474) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.882 ( 0.071) | 1.412 ( 0.493) | 0.67- 0.63 | 44 | 1.072 ( 0.065) | 0.865 ( 0.062) | 1.474 ( 0.593) | 0.63- 0.59 | 45 | 1.009 ( 0.080) | 0.806 ( 0.036) | 1.283 ( 0.494) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 441 | 1.063 ( 0.108) | 1.003 ( 0.281) | 1.320 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb PROFFITPEAK info: 322 peaks in the peak location table UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) UB - matrix: -0.070287 0.031186 0.088440 ( 0.000314 0.000269 0.000113 ) -0.069107 -0.065287 -0.010646 ( 0.000222 0.000191 0.000080 ) 0.108397 -0.152515 0.116232 ( 0.000344 0.000295 0.000124 ) M - matrix: 0.021466 -0.014212 0.007119 ( 0.000092 0.000068 0.000051 ) -0.014212 0.028496 -0.014274 ( 0.000068 0.000095 0.000046 ) 0.007119 -0.014274 0.021445 ( 0.000051 0.000046 0.000035 ) unit cell: 5.915(13) 5.932(13) 5.933(11) 59.9(2) 90.00(17) 60.2(2) V = 147.5(4) UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) UB - matrix: -0.070287 0.031186 0.088440 ( 0.000314 0.000269 0.000113 ) -0.069107 -0.065287 -0.010646 ( 0.000222 0.000191 0.000080 ) 0.108397 -0.152515 0.116232 ( 0.000344 0.000295 0.000124 ) M - matrix: 0.021466 -0.014212 0.007119 ( 0.000092 0.000068 0.000051 ) -0.014212 0.028496 -0.014274 ( 0.000068 0.000095 0.000046 ) 0.007119 -0.014274 0.021445 ( 0.000051 0.000046 0.000035 ) unit cell: 5.915(13) 5.932(13) 5.933(11) 59.9(2) 90.00(17) 60.2(2) V = 147.5(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070009 0.030942 0.088493 ( 0.000294 0.000253 0.000106 ) -0.068515 -0.065471 -0.010587 ( 0.000205 0.000176 0.000074 ) 0.108519 -0.152259 0.116025 ( 0.000325 0.000279 0.000117 ) M - matrix: 0.021372 -0.014203 0.007121 ( 0.000086 0.000064 0.000048 ) -0.014203 0.028427 -0.014235 ( 0.000064 0.000089 0.000044 ) 0.007121 -0.014235 0.021405 ( 0.000048 0.000044 0.000033 ) UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) unit cell: 5.937(12) 5.943(12) 5.936(10) 60.0(2) 90.03(16) 60.1(2) V = 148.3(4) UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) UB - matrix: -0.070009 0.030942 0.088493 ( 0.000294 0.000253 0.000106 ) -0.068515 -0.065471 -0.010587 ( 0.000205 0.000176 0.000074 ) 0.108519 -0.152259 0.116025 ( 0.000325 0.000279 0.000117 ) M - matrix: 0.021372 -0.014203 0.007121 ( 0.000086 0.000064 0.000048 ) -0.014203 0.028427 -0.014235 ( 0.000064 0.000089 0.000044 ) 0.007121 -0.014235 0.021405 ( 0.000048 0.000044 0.000033 ) unit cell: 5.937(12) 5.943(12) 5.936(10) 60.0(2) 90.03(16) 60.1(2) V = 148.3(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070009 0.030942 0.088493 ( 0.000294 0.000253 0.000106 ) -0.068515 -0.065471 -0.010587 ( 0.000205 0.000176 0.000074 ) 0.108519 -0.152259 0.116025 ( 0.000325 0.000279 0.000117 ) M - matrix: 0.021372 -0.014203 0.007121 ( 0.000086 0.000064 0.000048 ) -0.014203 0.028427 -0.014235 ( 0.000064 0.000089 0.000044 ) 0.007121 -0.014235 0.021405 ( 0.000048 0.000044 0.000033 ) UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) unit cell: 5.937(12) 5.943(12) 5.936(10) 60.0(2) 90.03(16) 60.1(2) V = 148.3(4) 149 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Run 2 Omega scan: (-103.000 - -78.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.050) HKL list info: 271 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070009 0.030942 0.088493 ( 0.000294 0.000253 0.000106 ) -0.068515 -0.065471 -0.010587 ( 0.000205 0.000176 0.000074 ) 0.108519 -0.152259 0.116025 ( 0.000325 0.000279 0.000117 ) M - matrix: 0.021372 -0.014203 0.007121 ( 0.000086 0.000064 0.000048 ) -0.014203 0.028427 -0.014235 ( 0.000064 0.000089 0.000044 ) 0.007121 -0.014235 0.021405 ( 0.000048 0.000044 0.000033 ) UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) unit cell: 5.937(12) 5.943(12) 5.936(10) 60.0(2) 90.03(16) 60.1(2) V = 148.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 138 obs out of 149 (total:149,skipped:0) (92.62%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb 1 of 92 peaks identified as outliers and rejected 91 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 91 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 91 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.28 | 9 | 1.002 ( 0.087) | 1.071 ( 0.091) | 0.925 ( 0.417) | 1.28- 1.09 | 9 | 1.019 ( 0.096) | 1.104 ( 0.115) | 0.869 ( 0.306) | 1.09- 0.92 | 9 | 1.040 ( 0.083) | 1.101 ( 0.146) | 1.057 ( 0.355) | 0.92- 0.84 | 9 | 1.028 ( 0.075) | 1.066 ( 0.146) | 1.077 ( 0.352) | 0.84- 0.78 | 9 | 0.988 ( 0.079) | 1.049 ( 0.135) | 0.949 ( 0.172) | 0.78- 0.73 | 9 | 1.013 ( 0.033) | 1.124 ( 0.161) | 1.036 ( 0.397) | 0.73- 0.69 | 9 | 0.973 ( 0.052) | 0.958 ( 0.119) | 1.041 ( 0.430) | 0.69- 0.67 | 9 | 0.974 ( 0.029) | 0.889 ( 0.059) | 1.346 ( 0.412) | 0.67- 0.63 | 9 | 0.944 ( 0.039) | 0.908 ( 0.106) | 1.189 ( 0.357) | 0.63- 0.59 | 10 | 0.907 ( 0.036) | 0.854 ( 0.088) | 1.059 ( 0.341) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.59 | 91 | 0.988 ( 0.076) | 1.011 ( 0.154) | 1.055 ( 0.383) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) UB - matrix: -0.069870 0.030679 0.088771 ( 0.000156 0.000131 0.000062 ) -0.067650 -0.066238 -0.010347 ( 0.000117 0.000098 0.000046 ) 0.109234 -0.152590 0.116162 ( 0.000131 0.000110 0.000052 ) M - matrix: 0.021391 -0.014331 0.007186 ( 0.000039 0.000027 0.000022 ) -0.014331 0.028612 -0.014316 ( 0.000027 0.000037 0.000019 ) 0.007186 -0.014316 0.021481 ( 0.000022 0.000019 0.000016 ) unit cell: 5.950(6) 5.936(6) 5.928(5) 60.06(11) 90.06(8) 59.91(11) V = 147.9(2) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: -0.070317 0.031106 0.088684 ( 0.000146 0.000123 0.000058 ) -0.068474 -0.065930 -0.010375 ( 0.000073 0.000062 0.000029 ) 0.109047 -0.152787 0.116289 ( 0.000120 0.000101 0.000047 ) M - matrix: 0.021524 -0.014334 0.007155 ( 0.000035 0.000024 0.000020 ) -0.014334 0.028658 -0.014325 ( 0.000024 0.000033 0.000018 ) 0.007155 -0.014325 0.021496 ( 0.000020 0.000018 0.000015 ) UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) unit cell: 5.920(5) 5.925(5) 5.924(5) 59.99(9) 89.96(7) 59.99(8) V = 146.94(16) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -78.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.978) HKL list info: 268 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb 1 of 91 peaks identified as outliers and rejected 90 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 90 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 90 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.27 | 9 | 1.004 ( 0.086) | 1.072 ( 0.091) | 0.927 ( 0.414) | 1.27- 1.09 | 9 | 1.048 ( 0.090) | 1.128 ( 0.097) | 0.919 ( 0.283) | 1.09- 0.92 | 9 | 1.009 ( 0.076) | 1.053 ( 0.145) | 1.134 ( 0.423) | 0.92- 0.84 | 9 | 1.053 ( 0.073) | 1.109 ( 0.144) | 0.991 ( 0.219) | 0.84- 0.78 | 9 | 0.984 ( 0.076) | 1.061 ( 0.154) | 0.949 ( 0.174) | 0.75- 0.73 | 9 | 0.994 ( 0.048) | 1.121 ( 0.144) | 1.003 ( 0.424) | 0.72- 0.69 | 9 | 0.985 ( 0.041) | 0.922 ( 0.079) | 1.023 ( 0.388) | 0.68- 0.66 | 9 | 0.973 ( 0.037) | 0.913 ( 0.109) | 1.301 ( 0.399) | 0.64- 0.62 | 9 | 0.942 ( 0.030) | 0.863 ( 0.040) | 1.308 ( 0.404) | 0.62- 0.59 | 9 | 0.896 ( 0.031) | 0.858 ( 0.094) | 1.083 ( 0.353) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.59 | 90 | 0.989 ( 0.077) | 1.010 ( 0.155) | 1.064 ( 0.384) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-14.1 | 53 | 1.130 ( 0.062) | 1.221 ( 0.316) | 1.429 ( 2.059) | 14.2-19.7 | 53 | 1.120 ( 0.064) | 1.153 ( 0.217) | 1.278 ( 0.572) | 19.8-23.8 | 53 | 1.109 ( 0.084) | 1.157 ( 0.341) | 1.272 ( 0.505) | 23.8-28.2 | 53 | 1.079 ( 0.096) | 1.125 ( 0.392) | 1.295 ( 0.502) | 28.4-31.3 | 53 | 1.047 ( 0.096) | 0.969 ( 0.099) | 1.256 ( 0.480) | 31.4-34.5 | 53 | 1.048 ( 0.092) | 0.947 ( 0.129) | 1.260 ( 0.505) | 34.6-37.3 | 53 | 1.019 ( 0.087) | 0.899 ( 0.097) | 1.332 ( 0.534) | 37.4-39.8 | 53 | 0.986 ( 0.119) | 0.900 ( 0.198) | 1.248 ( 0.576) | 39.9-42.8 | 53 | 0.976 ( 0.104) | 0.852 ( 0.101) | 1.190 ( 0.498) | 42.8-49.7 | 54 | 0.990 ( 0.099) | 0.823 ( 0.072) | 1.207 ( 0.472) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.7 | 531 | 1.050 ( 0.107) | 1.004 ( 0.264) | 1.277 ( 0.817) | Fitted profile normalization line parameters e1 dimension: a=-0.0035 b=1.13 e2 dimension: a=-0.0101 b=1.28 e3 dimension: a=0.0041 b=0.95 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 4108 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 707000 Maximum peak integral for reflections I/sig<= 10000 - raw: 8417059 lp-corr: 2435941 PROFFITPEAK - Finished at Tue Mar 27 13:37:41 2018 PROFFITMAIN - Started at Tue Mar 27 13:37:41 2018 OTKP changes: 531 1 2 2 OTKP changes: 531 1 2 2 UB - matrix: -0.070281 0.030970 0.088810 ( 0.000026 0.000025 0.000015 ) -0.068305 -0.066131 -0.010667 ( 0.000022 0.000021 0.000013 ) 0.109332 -0.153257 0.116361 ( 0.000022 0.000022 0.000013 ) M - matrix: 0.021558 -0.014415 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028820 -0.014377 ( 0.000005 0.000007 0.000004 ) 0.007209 -0.014377 0.021541 ( 0.000004 0.000004 0.000004 ) UB fit with 531 obs out of 531 (total:531,skipped:0) (100.00%) unit cell: 5.9215(12) 5.9095(12) 5.9173(10) 60.07(2) 90.070(16) 59.96(2) V = 146.40(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070144 0.030731 0.088844 ( 0.000027 0.000027 0.000016 ) -0.068157 -0.066108 -0.010667 ( 0.000024 0.000024 0.000014 ) 0.109147 -0.153130 0.116133 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021479 -0.014364 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014364 0.028763 -0.014348 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014348 0.021494 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9302(14) 5.9149(14) 5.9238(11) 60.04(2) 90.023(17) 59.97(2) V = 146.92(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070299 0.030881 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068358 -0.066105 -0.010681 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153228 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014400 0.007198 ( 0.000007 0.000005 0.000004 ) -0.014400 0.028802 -0.014370 ( 0.000005 0.000008 0.000004 ) 0.007198 -0.014370 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9187(13) 5.9105(13) 5.9210(10) 60.04(2) 90.055(16) 59.99(2) V = 146.46(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.835) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070299 0.030881 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068358 -0.066105 -0.010681 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153228 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014400 0.007198 ( 0.000007 0.000005 0.000004 ) -0.014400 0.028802 -0.014370 ( 0.000005 0.000008 0.000004 ) 0.007198 -0.014370 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9187(13) 5.9105(13) 5.9210(10) 60.04(2) 90.055(16) 59.99(2) V = 146.46(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070299 0.030881 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068358 -0.066105 -0.010681 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153228 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014400 0.007198 ( 0.000007 0.000005 0.000004 ) -0.014400 0.028802 -0.014370 ( 0.000005 0.000008 0.000004 ) 0.007198 -0.014370 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9187(13) 5.9105(13) 5.9210(10) 60.04(2) 90.055(16) 59.99(2) V = 146.46(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) UB - matrix: -0.070442 0.031209 0.088658 ( 0.000149 0.000125 0.000058 ) -0.068625 -0.065869 -0.010382 ( 0.000077 0.000065 0.000030 ) 0.108997 -0.152807 0.116290 ( 0.000121 0.000102 0.000047 ) M - matrix: 0.021552 -0.014334 0.007142 ( 0.000035 0.000025 0.000021 ) -0.014334 0.028663 -0.014319 ( 0.000025 0.000033 0.000018 ) 0.007142 -0.014319 0.021491 ( 0.000021 0.000018 0.000015 ) unit cell: 5.914(5) 5.923(5) 5.924(5) 59.98(9) 89.93(7) 60.00(9) V = 146.77(17) OTKP changes: 90 1 1 1 OTKP changes: 90 1 1 1 UB - matrix: -0.070377 0.031129 0.088720 ( 0.000149 0.000125 0.000058 ) -0.068517 -0.065923 -0.010370 ( 0.000073 0.000061 0.000029 ) 0.109052 -0.152841 0.116293 ( 0.000122 0.000103 0.000048 ) M - matrix: 0.021540 -0.014341 0.007149 ( 0.000035 0.000025 0.000021 ) -0.014341 0.028675 -0.014329 ( 0.000025 0.000033 0.000018 ) 0.007149 -0.014329 0.021503 ( 0.000021 0.000018 0.000015 ) UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) unit cell: 5.918(5) 5.923(5) 5.923(5) 59.98(9) 89.93(7) 59.98(8) V = 146.80(17) Run 2 Omega scan: (-103.000 - -78.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.964) HKL list info: 259 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070377 0.031129 0.088720 ( 0.000149 0.000125 0.000058 ) -0.068517 -0.065923 -0.010370 ( 0.000073 0.000061 0.000029 ) 0.109052 -0.152841 0.116293 ( 0.000122 0.000103 0.000048 ) M - matrix: 0.021540 -0.014341 0.007149 ( 0.000035 0.000025 0.000021 ) -0.014341 0.028675 -0.014329 ( 0.000025 0.000033 0.000018 ) 0.007149 -0.014329 0.021503 ( 0.000021 0.000018 0.000015 ) UB fit with 90 obs out of 90 (total:90,skipped:0) (100.00%) unit cell: 5.918(5) 5.923(5) 5.923(5) 59.98(9) 89.93(7) 59.98(8) V = 146.80(17) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070269 0.030931 0.088790 ( 0.000025 0.000024 0.000015 ) -0.068308 -0.066070 -0.010659 ( 0.000023 0.000022 0.000013 ) 0.109337 -0.153169 0.116289 ( 0.000023 0.000022 0.000013 ) M - matrix: 0.021558 -0.014407 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014407 0.028783 -0.014361 ( 0.000005 0.000007 0.000004 ) 0.007204 -0.014361 0.021520 ( 0.000004 0.000004 0.000004 ) UB fit with 531 obs out of 531 (total:531,skipped:0) (100.00%) unit cell: 5.9218(13) 5.9138(13) 5.9201(10) 60.07(2) 90.060(16) 59.95(2) V = 146.57(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 33 reflections under beam stop or inside a detector rejection region 7 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof 760 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:37:43 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.835) Run 2 Omega scan: (-103.000 - -78.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.964) PROFFIT INFO: signal sum: min=271.0000 max=20215992.0000 PROFFIT INFO: signal sum lp corr: min=631.2479 max=2947344.9934 PROFFIT INFO: background sum: min=1224.0000 max=9330.0000 PROFFIT INFO: background sum sig2: min=564.0000 max=6634.0000 PROFFIT INFO: num of signal pixels: min=53 max=545 PROFFIT INFO: Inet: min=1009.9967 max=4715752.0000 PROFFIT INFO: sig(Inet): min=182.7319 max=47422.4414 PROFFIT INFO: Inet/sig(Inet): min=1.08 max=228.50 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 24 70 162 179 287 494 686 760 Percent 0.0 0.0 0.5 3.2 9.2 21.3 23.6 37.8 65.0 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 760 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 760 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4715752- 1369337 76 2134065.00 128.13 100.00 1337048- 758890 76 985792.36 109.07 100.00 755040- 292711 76 476631.87 97.57 100.00 291748- 183563 76 225335.07 70.94 100.00 183360- 145370 76 166603.58 54.81 100.00 145072- 106111 76 120683.22 35.93 100.00 105700- 80301 76 91987.47 30.55 100.00 80255- 5724 76 39974.69 18.76 100.00 5664- 3408 76 4332.01 5.39 97.37 3398- 1010 76 2631.56 4.10 71.05 ------------------------------------------------------------------------------------ 4715752- 1010 760 424803.68 55.53 96.84 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 76 837694.44 88.72 100.00 1.28- 1.03 76 581550.97 64.13 97.37 1.03- 0.90 76 545133.63 61.85 98.68 0.90- 0.81 76 419125.42 58.46 97.37 0.81- 0.74 76 446363.71 63.10 97.37 0.74- 0.67 76 436764.42 61.66 98.68 0.67- 0.62 76 182923.56 35.76 93.42 0.61- 0.57 76 368018.12 51.99 94.74 0.57- 0.51 76 221145.26 35.90 93.42 0.51- 0.40 76 209317.28 33.67 97.37 ------------------------------------------------------------------------------------ 5.26- 0.40 760 424803.68 55.53 96.84 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:37:43 2018 Sorting 760 observations 170 unique observations with > 7.00 F2/sig(F2) 760 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 24 134 Total number of frames 134 Maximum number of 170 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 760 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 24 134 Total number of frames 134 604 observations > 7.00 F2/sig(F2) 604 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 24 134 Total number of frames 134 Frame #58 of 134 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 604 removed 89 = 515, unique = 150) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 515 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 24 134 Total number of frames 134 Frame #23 of 134 skipped from refinement Frame #58 of 134 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 150 unique data precomputed (should be 150) 150 unique data with 515 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.4 (Out of 515 removed 0 = 515, unique = 150) 150 unique data precomputed (should be 150) 150 unique data with 515 observations RMS deviation of equivalent data = 0.64497 Rint = 0.58597 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.55581, wR= 4.29571 Trying model 1 (ne=2, no=0)... Results: Rint= 0.86187, wR= 1.65049, Acormin=-0.335, Acormax=1.403, Acor_av=0.340 F test: Probability=0.000, F= 0.410 Trying model 2 (ne=2, no=1)... Results: Rint= 0.85437, wR= 2.58243, Acormin=-0.456, Acormax=1.257, Acor_av=0.160 F test: Probability=0.000, F= 0.414 Trying model 3 (ne=4, no=0)... Results: Rint= 0.86583, wR= 2.20230, Acormin=-0.413, Acormax=1.790, Acor_av=0.147 F test: Probability=0.000, F= 0.396 Trying model 4 (ne=4, no=1)... Results: Rint= 0.88646, wR= 1.56311, Acormin=-0.702, Acormax=1.324, Acor_av=0.073 F test: Probability=0.000, F= 0.375 Trying model 5 (ne=4, no=3)... Results: Rint= 0.90543, wR= 2.54082, Acormin=-0.242, Acormax=0.359, Acor_av=0.011 F test: Probability=0.000, F= 0.352 Trying model 6 (ne=6, no=0)... Results: Rint= 0.96140, wR= 2.12196, Acormin=-0.453, Acormax=2.448, Acor_av=0.074 F test: Probability=0.000, F= 0.309 Trying model 7 (ne=6, no=1)... Results: Rint= 0.89057, wR= 1.84057, Acormin=-0.943, Acormax=1.429, Acor_av=0.042 F test: Probability=0.000, F= 0.357 Trying model 8 (ne=6, no=3)... Results: Rint= 0.92220, wR= 3.34446, Acormin=-0.270, Acormax=0.271, Acor_av=0.006 F test: Probability=0.000, F= 0.326 Trying model 9 (ne=6, no=5)... Results: Rint= 0.86884, wR= 2.08876, Acormin=-0.055, Acormax=0.119, Acor_av=0.002 F test: Probability=0.000, F= 0.355 Trying model 10 (ne=8, no=0)... Results: Rint= 0.82660, wR= 2.42046, Acormin=-0.513, Acormax=1.666, Acor_av=0.004 F test: Probability=0.000, F= 0.397 Trying model 11 (ne=8, no=1)... Results: Rint= 0.87993, wR= 1.53449, Acormin=-0.462, Acormax=0.852, Acor_av=0.007 F test: Probability=0.000, F= 0.347 Trying model 12 (ne=8, no=3)... Results: Rint= 0.84113, wR= 1.88335, Acormin=-0.035, Acormax=0.054, Acor_av=0.000 F test: Probability=0.000, F= 0.371 Trying model 13 (ne=8, no=5)... Results: Rint= 0.89232, wR= 1.25973, Acormin=-0.023, Acormax=0.058, Acor_av=0.001 F test: Probability=0.000, F= 0.318 Trying model 14 (ne=8, no=7)... Results: Rint= 0.59428, wR= 1.97147, Acormin=-0.004, Acormax=0.011, Acor_av=0.002 F test: Probability=0.000, F= 0.681 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.73529 There are 132 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.64497 Using Levenberg-Marquardt: 0.00010 New wR= 0.60935 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.58597 with corrections 0.54377 Rint for all data: 0.73529 with corrections 0.70819 1 observations identified as outliers and rejected Cycle 2 wR= 0.60728 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.59744 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.57745 with corrections 0.56144 Rint for all data: 0.73529 with corrections 0.72629 3 observations identified as outliers and rejected Cycle 3 wR= 0.58902 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57638 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55581 with corrections 0.53374 Rint for all data: 0.73529 with corrections 0.72604 1 observations identified as outliers and rejected Cycle 4 wR= 0.57126 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56567 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.54182 Rint for all data: 0.73529 with corrections 0.73274 0 observations identified as outliers and rejected Cycle 5 wR= 0.56567 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.56339 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.55524 Rint for all data: 0.73529 with corrections 0.74173 0 observations identified as outliers and rejected Final wR= 0.56339 Final frame scales: Min= 0.9062 Max= 18.1035 Final absorption correction factors: Amin= 0.1421 Amax= 3.3717 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 132 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.87481 Using Levenberg-Marquardt: 0.00010 New wR= 0.64240 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.90015 Rint for all data: 0.73529 with corrections 0.98228 0 observations identified as outliers and rejected Cycle 2 wR= 0.64240 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.63933 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.89051 Rint for all data: 0.73529 with corrections 0.97730 0 observations identified as outliers and rejected Cycle 3 wR= 0.63933 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.63639 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.88511 Rint for all data: 0.73529 with corrections 0.97416 0 observations identified as outliers and rejected Cycle 4 wR= 0.63639 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.63359 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.88180 Rint for all data: 0.73529 with corrections 0.97225 0 observations identified as outliers and rejected Cycle 5 wR= 0.63359 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.63095 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.55263 with corrections 0.87984 Rint for all data: 0.73529 with corrections 0.97125 0 observations identified as outliers and rejected Final wR= 0.63095 Frame scales out of range! Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 119 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 118 pars with 7021 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.91371 Using Levenberg-Marquardt: 0.00010 New wR= 0.64068 There are 7 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.59204 Rint for all data: 0.73529 with corrections 0.75698 0 observations identified as outliers and rejected Cycle 2 wR= 0.62110 Using Levenberg-Marquardt: 0.00001 New wR= 0.78975 Using Levenberg-Marquardt: 0.00010 New wR= 0.80511 Using Levenberg-Marquardt: 0.00100 New wR= 0.82310 Using Levenberg-Marquardt: 0.01000 New wR= 0.58780 There are 7 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.57614 Rint for all data: 0.73529 with corrections 0.74742 0 observations identified as outliers and rejected Cycle 3 wR= 0.58910 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.58758 There are 7 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.57009 Rint for all data: 0.73529 with corrections 0.74251 0 observations identified as outliers and rejected Cycle 4 wR= 0.58852 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.58720 There are 7 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.56755 Rint for all data: 0.73529 with corrections 0.74004 0 observations identified as outliers and rejected Cycle 5 wR= 0.58801 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.58687 There are 7 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.56669 Rint for all data: 0.73529 with corrections 0.73924 0 observations identified as outliers and rejected Final wR= 0.58687 Final frame scales: Min= 0.5169 Max= 10.3288 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 104 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 103 pars with 5356 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.83065 Using Levenberg-Marquardt: 0.00010 New wR= 0.65493 There are 11 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.54704 Rint for all data: 0.73529 with corrections 0.72362 0 observations identified as outliers and rejected Cycle 2 wR= 0.61392 Using Levenberg-Marquardt: 0.00001 New wR= 0.59744 There are 11 clusters with unrefined scales (size 1-7) Rint for refined data: 0.55263 with corrections 0.52758 Rint for all data: 0.73529 with corrections 0.71400 1 observations identified as outliers and rejected Cycle 3 wR= 0.59724 Using Levenberg-Marquardt: 0.00000 New wR= 0.59821 Using Levenberg-Marquardt: 0.00001 New wR= 0.59821 Using Levenberg-Marquardt: 0.00010 New wR= 0.59818 Using Levenberg-Marquardt: 0.00100 New wR= 0.59792 Using Levenberg-Marquardt: 0.01000 New wR= 0.59666 There are 11 clusters with unrefined scales (size 1-7) Rint for refined data: 0.54926 with corrections 0.52064 Rint for all data: 0.73529 with corrections 0.71636 Final wR= 0.59666 Final frame scales: Min= 1.0000 Max= 3.3297 1 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=916.7965 max=5191814.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.8633 max=52792.1484 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/108 759 reflections read from tmp file 615 reflections are rejected (491 as outliers, 124 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 56 8 2 Initial Chi^2= 0.77080 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.06926 Current error model SIG(F2)^2 = 294.00*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 314.37*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 314.37*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5191814- 1261319 75 2135569.10 89.67 100.00 1260675- 704743 75 980425.26 42.39 100.00 704681- 308337 75 471383.37 38.91 100.00 307070- 183711 75 237665.78 27.39 100.00 183631- 142369 75 161566.88 20.73 100.00 141875- 105376 75 125273.37 15.66 100.00 104730- 75948 75 89298.04 11.89 100.00 75368- 6092 75 44809.81 8.42 88.00 5996- 3338 75 4419.06 3.06 28.00 3331- 917 84 2527.01 2.64 20.24 ------------------------------------------------------------------------------------ 5191814- 917 759 420280.72 25.80 82.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 75 935871.71 59.09 97.33 1.28- 1.03 75 569342.01 36.34 92.00 1.03- 0.90 75 527823.36 31.66 89.33 0.90- 0.81 75 385863.44 23.38 77.33 0.81- 0.74 75 423995.42 24.77 85.33 0.74- 0.67 75 405635.01 23.22 77.33 0.67- 0.62 75 214120.53 15.13 77.33 0.62- 0.57 75 353667.67 19.04 82.67 0.57- 0.52 75 202552.54 14.06 76.00 0.52- 0.40 84 209258.25 12.83 75.00 ------------------------------------------------------------------------------------ 5.26- 0.40 759 420280.72 25.80 82.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 75 935871.71 59.09 97.33 5.26- 1.03 150 752606.86 47.72 94.67 5.26- 0.90 225 677679.02 42.36 92.89 5.26- 0.81 300 604725.13 37.62 89.00 5.26- 0.74 375 568579.19 35.05 88.27 5.26- 0.67 450 541421.82 33.08 86.44 5.26- 0.62 525 494664.50 30.51 85.14 5.26- 0.57 600 477039.89 29.08 84.83 5.26- 0.52 675 446541.30 27.41 83.85 5.26- 0.40 759 420280.72 25.80 82.87 ------------------------------------------------------------------------------------ 5.26- 0.40 759 420280.72 25.80 82.87 Scale applied to data: s=0.192611 (maximum obs:5191814.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.713; Rsigma 0.025: data 759 -> merged 265 With outlier rejection... Rint 0.554; Rsigma 0.027: data 631 -> merged 265 Rejected total: 128, method kkm 126, method Blessing 2 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404383, 5.272505 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 2.53 100.00 38 1.46 - 1.12 15 15 4.67 100.00 70 1.08 - 0.96 15 15 4.13 100.00 62 0.96 - 0.86 15 15 3.93 100.00 59 0.86 - 0.79 15 15 3.00 100.00 45 0.79 - 0.73 15 15 2.87 100.00 43 0.73 - 0.69 15 15 2.40 100.00 36 0.69 - 0.65 15 15 2.27 100.00 34 0.65 - 0.63 15 15 1.93 100.00 29 0.63 - 0.60 21 21 2.00 100.00 42 --------------------------------------------------------------- 5.92 - 0.60 156 156 2.94 100.00 458 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:37:43 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921826 5.913776 5.920137 60.0687 90.0603 59.9531 631 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 311 333 304 328 474 425 431 631 N (int>3sigma) = 0 250 333 243 265 413 347 351 513 Mean intensity = 0.0 59.5 31.8 59.6 66.7 49.8 71.1 65.2 67.3 Mean int/sigma = 0.0 22.3 21.0 22.7 23.2 22.0 24.1 23.2 23.3 Lattice type: P chosen Volume: 146.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.917 90.05 119.94 119.91 Niggli form: a.a = 34.971 b.b = 34.973 c.c = 35.007 b.c = -0.031 a.c = -17.465 a.b = -17.438 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.139 CUBIC F-lattice R(int) = 0.150 [ 481] Vol = 586.3 Cell: 8.369 8.378 8.362 90.09 89.97 89.98 Volume: 586.29 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.125 RHOMBOHEDRAL R-lattice R(int) = 0.134 [ 313] Vol = 439.7 Cell: 5.922 5.914 14.505 90.00 90.08 120.05 Volume: 439.72 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.125 RHOMBOHEDRAL R-lattice R(int) = 0.132 [ 84] Vol = 439.7 Trigonal Cell: 5.922 5.914 14.505 90.00 90.08 120.05 Volume: 439.72 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.121 [ 300] Vol = 293.1 Cell: 5.920 5.922 8.362 89.96 89.91 89.94 Volume: 293.14 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.127 TETRAGONAL I-lattice R(int) = 0.121 [ 300] Vol = 293.1 Cell: 5.922 5.920 8.362 90.09 90.04 89.94 Volume: 293.14 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.138 [ 327] Vol = 293.1 Cell: 5.922 5.920 8.362 89.91 89.96 89.94 Volume: 293.14 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.132 [ 260] Vol = 293.1 Cell: 5.914 8.369 5.923 89.99 89.89 90.03 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.121 [ 196] Vol = 293.1 Cell: 5.920 5.922 8.362 90.04 90.09 89.94 Volume: 293.14 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.094 MONOCLINIC I-lattice R(int) = 0.119 [ 137] Vol = 293.1 Cell: 5.914 5.923 8.369 90.01 90.03 90.11 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.040 MONOCLINIC I-lattice R(int) = 0.095 [ 137] Vol = 293.1 Cell: 5.914 8.369 5.923 89.99 90.11 89.97 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.052 MONOCLINIC I-lattice R(int) = 0.142 [ 133] Vol = 293.1 Cell: 8.369 5.914 5.923 90.11 90.01 90.03 Volume: 293.14 Matrix:-1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.103 MONOCLINIC C-lattice R(int) = 0.111 [ 176] Vol = 293.1 Cell: 10.252 5.914 5.917 90.05 125.20 89.91 Volume: 293.14 Matrix:-2.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 27] Vol = 146.6 Cell: 5.914 5.914 5.917 90.05 119.94 119.91 Volume: 146.57 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 333 0 432 418 631 N (int>3sigma) = 0 0 0 0 333 0 350 342 513 Mean intensity = 0.0 0.0 0.0 0.0 31.8 0.0 67.2 72.1 67.3 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 23.2 23.9 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.082 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 50 151 N I>3s 8 8 28 151 0.8 0.8 0.8 37.3 6.2 6.2 3.6 25.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.150 450 Fd-3m 1 1 227 C N N N N 37 2284 0.157 487 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.369125 8.377938 8.361698 90.0919 89.9716 89.9837 ZERR 1.00 0.000432 0.002729 0.006009 0.0030 0.0197 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4618628- 895389 82 60 26 2.3 1368346.69 57.02 0.392 0.267 886461- 579416 93 85 26 3.3 698399.41 37.54 0.797 0.668 568966- 421971 85 68 26 2.6 365152.94 24.48 0.744 0.712 420943- 305881 87 67 26 2.6 242391.63 23.39 0.506 0.550 305803- 188954 101 80 26 3.1 188042.33 20.54 0.485 0.544 188136- 132850 81 61 26 2.3 137247.61 18.82 0.337 0.237 132445- 96805 67 54 26 2.1 120110.48 14.62 0.333 0.224 96787- 76764 64 62 26 2.4 84053.40 11.75 0.409 0.318 75948- 35785 51 47 26 1.8 58070.90 8.73 0.443 0.365 28347- 1498 48 47 31 1.5 4140.13 2.91 0.222 0.234 ------------------------------------------------------------------------------------------- 4618628- 1498 759 631 265 2.4 349559.55 23.30 0.554 0.441 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.18 105 86 27 3.2 665943.94 46.55 0.491 0.345 0.013 1.15-0.89 137 119 26 4.6 434732.49 30.09 0.674 0.607 0.022 0.89-0.76 103 79 26 3.0 383985.47 22.60 0.574 0.329 0.028 0.75-0.69 85 69 26 2.7 267610.31 17.80 0.627 0.572 0.033 0.69-0.64 71 55 26 2.1 248334.34 17.08 0.382 0.368 0.036 0.63-0.60 67 54 27 2.0 252901.73 16.16 0.367 0.307 0.039 0.59-0.56 55 48 27 1.8 218378.19 13.44 0.556 0.561 0.042 0.56-0.52 43 38 26 1.5 257162.05 16.72 0.411 0.411 0.041 0.52-0.48 57 47 26 1.8 111078.74 10.55 0.589 0.606 0.064 0.48-0.40 36 36 28 1.3 277157.53 14.27 0.835 0.835 0.043 ------------------------------------------------------------------------------------------------------ inf-0.40 759 631 265 2.4 349559.55 23.30 0.554 0.441 0.027 inf-0.60 561 458 156 2.9 400910.02 26.89 0.559 0.421 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.18 86 27 27 100.0 3.2 665943.94 101.54 0.491 0.008 1.15-0.89 119 26 26 100.0 4.6 434732.49 78.96 0.674 0.013 0.89-0.76 79 26 26 100.0 3.0 383985.47 48.52 0.574 0.020 0.75-0.69 69 26 26 100.0 2.7 267610.31 37.78 0.627 0.024 0.69-0.64 55 26 26 100.0 2.1 248334.34 27.88 0.382 0.025 0.63-0.60 54 27 27 100.0 2.0 252901.73 25.99 0.367 0.028 0.59-0.56 48 32 27 84.4 1.8 218378.19 19.78 0.556 0.032 0.56-0.52 38 30 26 86.7 1.5 257162.05 23.22 0.411 0.029 0.52-0.48 47 66 26 39.4 1.8 111078.74 15.98 0.589 0.046 0.48-0.40 36 174 28 16.1 1.3 277157.53 17.62 0.835 0.043 -------------------------------------------------------------------------------------------- inf-0.40 631 460 265 57.6 2.4 349559.55 48.69 0.554 0.019 inf-0.60 458 156 156 100.0 2.9 400910.02 59.77 0.559 0.016 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: -0.024726 0.079529 0.015466 ( 0.000011 0.000011 0.000012 ) 0.072519 0.028825 -0.033035 ( 0.000010 0.000010 0.000011 ) -0.036228 0.003476 -0.076584 ( 0.000010 0.000010 0.000011 ) M - matrix: 0.007183 -0.000002 -0.000004 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007168 0.000012 ( 0.000001 0.000002 0.000001 ) -0.000004 0.000012 0.007196 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024726 0.079529 0.015466 ( 0.000011 0.000011 0.000012 ) 0.072519 0.028825 -0.033035 ( 0.000010 0.000010 0.000011 ) -0.036228 0.003476 -0.076584 ( 0.000010 0.000010 0.000011 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3691(10) 8.3779(11) 8.3617(10) 90.092(10) 89.972(10) 89.984(10) V = 586.29(13) unit cell: 8.3696(3) 8.3696(3) 8.3696(3) 90.0 90.0 90.0 V = 586.29(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.835) Run 2 Omega scan: (-103.000 - -78.000,25 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.964) PROFFIT INFO: signal sum: min=271.0000 max=20215992.0000 PROFFIT INFO: signal sum lp corr: min=631.2479 max=2947344.9934 PROFFIT INFO: background sum: min=1224.0000 max=9330.0000 PROFFIT INFO: background sum sig2: min=564.0000 max=6634.0000 PROFFIT INFO: num of signal pixels: min=53 max=545 PROFFIT INFO: Inet: min=1009.9967 max=4715752.0000 PROFFIT INFO: sig(Inet): min=182.7319 max=47422.4414 PROFFIT INFO: Inet/sig(Inet): min=1.08 max=228.50 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 48 140 324 358 574 988 1372 1520 Percent 0.0 0.0 0.5 3.2 9.2 21.3 23.6 37.8 65.0 90.3 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 760 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 760 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4715752- 1369337 76 2134065.00 128.13 100.00 1337048- 758890 76 985792.36 109.07 100.00 755040- 292711 76 476631.87 97.57 100.00 291748- 183563 76 225335.07 70.94 100.00 183360- 145370 76 166603.58 54.81 100.00 145072- 106111 76 120683.22 35.93 100.00 105700- 80301 76 91987.47 30.55 100.00 80255- 5724 76 39974.69 18.76 100.00 5664- 3408 76 4332.01 5.39 97.37 3398- 1010 76 2631.56 4.10 71.05 ------------------------------------------------------------------------------------ 4715752- 1010 760 424803.68 55.53 96.84 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 76 792297.44 83.68 100.00 1.32- 1.09 76 911826.11 78.11 100.00 1.09- 0.96 76 405590.43 65.41 100.00 0.96- 0.84 76 530592.45 74.95 97.37 0.84- 0.80 76 399318.17 61.03 100.00 0.80- 0.73 76 255461.07 43.06 100.00 0.73- 0.69 76 290344.42 42.66 86.84 0.69- 0.65 76 299349.92 45.35 97.37 0.65- 0.62 76 182286.29 31.37 90.79 0.62- 0.58 76 180970.51 29.64 96.05 ------------------------------------------------------------------------------------ 4.82- 0.58 760 424803.68 55.53 96.84 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:37:44 2018 Sorting 760 observations 78 unique observations with > 7.00 F2/sig(F2) 760 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 24 134 Total number of frames 134 Maximum number of 78 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 760 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 12 68 Total number of frames 68 604 observations > 7.00 F2/sig(F2) 604 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 12 68 Total number of frames 68 Removing 'redundancy=1' reflections Average redundancy: 7.4 (Out of 604 removed 7 = 597, unique = 81) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 597 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 12 68 Total number of frames 68 81 unique data precomputed (should be 81) 81 unique data with 597 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.4 (Out of 597 removed 0 = 597, unique = 81) 81 unique data precomputed (should be 81) 81 unique data with 597 observations RMS deviation of equivalent data = 0.08553 Rint = 0.07038 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.06723, wR= 0.09096 Trying model 1 (ne=2, no=0)... Results: Rint= 0.04752, wR= 0.06215, Acormin=0.848, Acormax=1.196, Acor_av=0.989 F test: Probability=1.000, F= 1.982 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04489, wR= 0.05851, Acormin=0.829, Acormax=1.213, Acor_av=1.004 F test: Probability=0.888, F= 1.114 Trying model 3 (ne=4, no=0)... Results: Rint= 0.03423, wR= 0.04768, Acormin=0.755, Acormax=1.192, Acor_av=0.954 F test: Probability=1.000, F= 1.893 Trying model 4 (ne=4, no=1)... Results: Rint= 0.02599, wR= 0.03705, Acormin=0.762, Acormax=1.241, Acor_av=0.966 F test: Probability=1.000, F= 1.724 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02419, wR= 0.03109, Acormin=0.755, Acormax=1.270, Acor_av=0.930 F test: Probability=0.925, F= 1.138 Trying model 6 (ne=6, no=0)... Results: Rint= 0.03085, wR= 0.03944, Acormin=0.701, Acormax=1.235, Acor_av=0.923 F test: Probability=0.000, F= 0.696 Trying model 7 (ne=6, no=1)... Results: Rint= 0.02311, wR= 0.03084, Acormin=0.756, Acormax=1.230, Acor_av=0.965 F test: Probability=0.989, F= 1.232 Trying model 8 (ne=6, no=3)... Results: Rint= 0.01944, wR= 0.02589, Acormin=0.775, Acormax=1.332, Acor_av=0.955 F test: Probability=1.000, F= 1.392 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01741, wR= 0.02287, Acormin=0.781, Acormax=1.320, Acor_av=0.968 F test: Probability=0.984, F= 1.219 Trying model 10 (ne=8, no=0)... Results: Rint= 0.02686, wR= 0.03305, Acormin=0.753, Acormax=1.242, Acor_av=0.957 F test: Probability=0.000, F= 0.423 Trying model 11 (ne=8, no=1)... Results: Rint= 0.01984, wR= 0.02617, Acormin=0.794, Acormax=1.268, Acor_av=0.967 F test: Probability=0.000, F= 0.771 Trying model 12 (ne=8, no=3)... Results: Rint= 0.01676, wR= 0.02234, Acormin=0.759, Acormax=1.287, Acor_av=0.968 F test: Probability=0.750, F= 1.065 Trying model 13 (ne=8, no=5)... Results: Rint= 0.01596, wR= 0.02124, Acormin=0.772, Acormax=1.309, Acor_av=0.971 F test: Probability=0.928, F= 1.146 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01524, wR= 0.02020, Acormin=0.768, Acormax=1.319, Acor_av=0.973 F test: Probability=0.980, F= 1.214 Final absorption model (ne=8, no=7): Rint= 0.01524, Acormin=0.768, Acormax=1.319, Acor_av=0.973 Combined refinement in use Rint: 0.07054 There are 68 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 147 pars with 10878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.08553 Using Levenberg-Marquardt: 0.00010 New wR= 0.01898 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07038 with corrections 0.01493 Rint for all data: 0.07054 with corrections 0.01517 0 observations identified as outliers and rejected Cycle 2 wR= 0.01898 Using Levenberg-Marquardt: 0.00001 New wR= 0.01796 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07038 with corrections 0.01412 Rint for all data: 0.07054 with corrections 0.01435 0 observations identified as outliers and rejected Cycle 3 wR= 0.01796 Using Levenberg-Marquardt: 0.00000 New wR= 0.01789 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07038 with corrections 0.01414 Rint for all data: 0.07054 with corrections 0.01437 0 observations identified as outliers and rejected Cycle 4 wR= 0.01789 Using Levenberg-Marquardt: 0.00000 New wR= 0.01788 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07038 with corrections 0.01419 Rint for all data: 0.07054 with corrections 0.01443 Final wR= 0.01788 Final frame scales: Min= 0.9363 Max= 1.0748 Final absorption correction factors: Amin= 0.7006 Amax= 1.1587 PROFFIT INFO: Inet (after scale3 abspack): min=980.7897 max=4861394.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=193.6058 max=45933.6523 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/109 760 reflections read from tmp file 19 reflections are rejected (13 as outliers, 6 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 11 6 10 11 13 8 10 26 Initial Chi^2= 0.26777 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.62463 Current error model SIG(F2)^2 = 93.81*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 246.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 246.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4861394- 1326146 76 2135026.56 102.38 100.00 1274989- 744892 76 970171.41 45.84 100.00 735634- 272687 76 484256.94 46.96 100.00 271389- 187416 76 222923.28 30.45 100.00 186520- 146723 76 167242.87 22.16 100.00 146474- 104630 76 115750.47 15.34 100.00 104204- 79711 76 92909.67 13.29 100.00 79479- 5597 76 40461.82 8.66 96.05 5542- 3346 76 4294.19 3.33 51.32 3342- 981 76 2639.38 2.88 35.53 ------------------------------------------------------------------------------------ 4861394- 981 760 423567.66 29.13 88.29 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 76 799765.84 64.36 96.05 1.32- 1.09 76 917376.89 57.04 100.00 1.09- 0.96 76 410343.37 29.59 92.11 0.96- 0.84 76 520356.78 31.64 86.84 0.84- 0.80 76 397130.28 25.90 94.74 0.80- 0.73 76 253403.53 18.49 89.47 0.73- 0.69 76 284779.46 18.34 77.63 0.69- 0.65 76 293191.23 19.32 86.84 0.65- 0.62 76 181116.76 13.65 82.89 0.62- 0.58 76 178212.45 12.96 76.32 ------------------------------------------------------------------------------------ 4.82- 0.58 760 423567.66 29.13 88.29 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 76 799765.84 64.36 96.05 4.82- 1.09 152 858571.36 60.70 98.03 4.82- 0.96 228 709162.03 50.33 96.05 4.82- 0.84 304 661960.72 45.66 93.75 4.82- 0.80 380 608994.63 41.71 93.95 4.82- 0.73 456 549729.45 37.84 93.20 4.82- 0.69 532 511879.45 35.05 90.98 4.82- 0.65 608 484543.42 33.08 90.46 4.82- 0.62 684 450829.35 30.93 89.62 4.82- 0.58 760 423567.66 29.13 88.29 ------------------------------------------------------------------------------------ 4.82- 0.58 760 423567.66 29.13 88.29 Scale applied to data: s=0.205702 (maximum obs:4861394.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.014; Rsigma 0.022: data 760 -> merged 106 With outlier rejection... Rint 0.013; Rsigma 0.023: data 753 -> merged 106 Rejected total: 7, method kkm 7, method Blessing 0 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585988, 4.832179 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 9 10 4.00 90.00 36 1.61 - 1.21 10 10 6.60 100.00 66 1.17 - 1.01 10 10 8.80 100.00 88 0.99 - 0.89 10 10 8.70 100.00 87 0.88 - 0.81 10 10 8.40 100.00 84 0.81 - 0.74 10 10 7.40 100.00 74 0.73 - 0.71 10 10 8.20 100.00 82 0.70 - 0.66 10 10 7.40 100.00 74 0.66 - 0.64 10 10 5.90 100.00 59 0.63 - 0.60 10 10 6.50 100.00 65 --------------------------------------------------------------- 5.92 - 0.60 99 100 7.22 99.00 715 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:37:43 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921826 5.913776 5.920137 60.0687 90.0603 59.9531 631 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.30 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 311 333 304 328 474 425 431 631 N (int>3sigma) = 0 250 333 243 265 413 347 351 513 Mean intensity = 0.0 59.5 31.8 59.6 66.7 49.8 71.1 65.2 67.3 Mean int/sigma = 0.0 22.3 21.0 22.7 23.2 22.0 24.1 23.2 23.3 Lattice type: P chosen Volume: 146.57 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.917 90.05 119.94 119.91 Niggli form: a.a = 34.971 b.b = 34.973 c.c = 35.007 b.c = -0.031 a.c = -17.465 a.b = -17.438 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.139 CUBIC F-lattice R(int) = 0.150 [ 481] Vol = 586.3 Cell: 8.369 8.378 8.362 90.09 89.97 89.98 Volume: 586.29 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.125 RHOMBOHEDRAL R-lattice R(int) = 0.134 [ 313] Vol = 439.7 Cell: 5.922 5.914 14.505 90.00 90.08 120.05 Volume: 439.72 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.125 RHOMBOHEDRAL R-lattice R(int) = 0.132 [ 84] Vol = 439.7 Trigonal Cell: 5.922 5.914 14.505 90.00 90.08 120.05 Volume: 439.72 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.121 [ 300] Vol = 293.1 Cell: 5.920 5.922 8.362 89.96 89.91 89.94 Volume: 293.14 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.127 TETRAGONAL I-lattice R(int) = 0.121 [ 300] Vol = 293.1 Cell: 5.922 5.920 8.362 90.09 90.04 89.94 Volume: 293.14 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.138 [ 327] Vol = 293.1 Cell: 5.922 5.920 8.362 89.91 89.96 89.94 Volume: 293.14 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.132 [ 260] Vol = 293.1 Cell: 5.914 8.369 5.923 89.99 89.89 90.03 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.037 MONOCLINIC I-lattice R(int) = 0.121 [ 196] Vol = 293.1 Cell: 5.920 5.922 8.362 90.04 90.09 89.94 Volume: 293.14 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.094 MONOCLINIC I-lattice R(int) = 0.119 [ 137] Vol = 293.1 Cell: 5.914 5.923 8.369 90.01 90.03 90.11 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.040 MONOCLINIC I-lattice R(int) = 0.095 [ 137] Vol = 293.1 Cell: 5.914 8.369 5.923 89.99 90.11 89.97 Volume: 293.14 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.052 MONOCLINIC I-lattice R(int) = 0.142 [ 133] Vol = 293.1 Cell: 8.369 5.914 5.923 90.11 90.01 90.03 Volume: 293.14 Matrix:-1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.103 MONOCLINIC C-lattice R(int) = 0.111 [ 176] Vol = 293.1 Cell: 10.252 5.914 5.917 90.05 125.20 89.91 Volume: 293.14 Matrix:-2.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.094 [ 27] Vol = 146.6 Cell: 5.914 5.914 5.917 90.05 119.94 119.91 Volume: 146.57 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 333 0 432 418 631 N (int>3sigma) = 0 0 0 0 333 0 350 342 513 Mean intensity = 0.0 0.0 0.0 0.0 31.8 0.0 67.2 72.1 67.3 Mean int/sigma = 0.0 0.0 0.0 0.0 21.0 0.0 23.2 23.9 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.082 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 8 8 50 151 N I>3s 8 8 28 151 0.8 0.8 0.8 37.3 6.2 6.2 3.6 25.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.150 450 Fd-3m 1 1 227 C N N N N 37 2284 0.157 487 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.369125 8.377938 8.361698 90.0919 89.9716 89.9837 ZERR 1.00 0.000432 0.002729 0.006009 0.0030 0.0197 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4787717- 642428 167 162 26 6.2 1430668.16 67.95 0.011 0.012 611242- 145951 217 216 26 8.3 258577.98 32.62 0.017 0.020 129579- 65623 184 184 26 7.1 96494.26 13.39 0.028 0.033 44119- 2317 192 191 28 6.8 5875.96 3.93 0.095 0.115 ------------------------------------------------------------------------------------------- 4787717- 2317 760 753 106 7.1 407036.31 28.24 0.013 0.014 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 179 172 26 6.6 734367.78 53.91 0.011 0.012 0.012 1.01-0.78 215 215 26 8.3 426474.21 27.65 0.010 0.011 0.022 0.78-0.66 202 202 26 7.8 300227.20 19.55 0.015 0.018 0.033 0.66-0.59 164 164 28 5.9 169812.37 12.81 0.025 0.030 0.047 ------------------------------------------------------------------------------------------------------ inf-0.59 760 753 106 7.1 407036.31 28.24 0.013 0.014 0.023 inf-0.60 720 713 98 7.3 422562.46 29.19 0.013 0.014 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 172 27 26 96.3 6.6 734367.78 143.60 0.011 0.005 1.01-0.78 215 26 26 100.0 8.3 426474.21 82.53 0.010 0.008 0.78-0.66 202 26 26 100.0 7.8 300227.20 57.38 0.015 0.012 0.66-0.59 164 31 28 90.3 5.9 169812.37 34.31 0.025 0.021 -------------------------------------------------------------------------------------------- inf-0.59 753 110 106 96.4 7.1 407036.31 79.23 0.013 0.008 inf-0.60 713 99 98 99.0 7.3 422562.46 82.06 0.013 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:44:32 2018) ID: 2932; threads 39; handles 878; mem 517384.00 (1237820.00)kB; time: 1w 4d 22h 50m 3s MEMORY INFO: Memory PF:246.0, Ph:429.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:505.3,peak PF: 697.1, WS: 296.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:248.0, Ph:429.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.0,peak PF: 697.1, WS: 298.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:44:32 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000025 0.000024 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000023 0.000022 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000022 0.000013 ) 5.91502 ( 0.00125 ) 5.91640 ( 0.00125 ) 5.92265 ( 0.00098 ) 60.05206 ( 0.02029 ) 89.98756 ( 0.01570 ) 60.01743 ( 0.02216 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:44:33 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000025 0.000024 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000023 0.000022 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000022 0.000013 ) M - matrix: 0.021558 -0.014407 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014407 0.028783 -0.014361 ( 0.000005 0.000007 0.000004 ) 0.007204 -0.014361 0.021520 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9150(13) 5.9164(13) 5.9227(10) 60.05(2) 89.988(16) 60.02(2) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 45 | 1.010 ( 0.079) | 0.807 ( 0.033) | 1.266 ( 0.501) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 441 | 1.063 ( 0.106) | 1.005 ( 0.289) | 1.295 ( 0.544) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb PROFFITPEAK info: 578 peaks in the peak location table UB fit with 262 obs out of 275 (total:275,skipped:0) (95.27%) UB - matrix: -0.070468 0.031397 0.088301 ( 0.000141 0.000105 0.000078 ) -0.069000 -0.065399 -0.010710 ( 0.000128 0.000095 0.000071 ) 0.108710 -0.152759 0.116177 ( 0.000169 0.000125 0.000093 ) M - matrix: 0.021545 -0.014306 0.007146 ( 0.000045 0.000032 0.000026 ) -0.014306 0.028598 -0.014274 ( 0.000032 0.000041 0.000023 ) 0.007146 -0.014274 0.021409 ( 0.000026 0.000023 0.000026 ) unit cell: 5.913(6) 5.925(7) 5.935(5) 60.02(11) 90.02(8) 60.06(12) V = 147.2(2) UB fit with 262 obs out of 275 (total:275,skipped:0) (95.27%) UB - matrix: -0.070468 0.031397 0.088301 ( 0.000141 0.000105 0.000078 ) -0.069000 -0.065399 -0.010710 ( 0.000128 0.000095 0.000071 ) 0.108710 -0.152759 0.116177 ( 0.000169 0.000125 0.000093 ) M - matrix: 0.021545 -0.014306 0.007146 ( 0.000045 0.000032 0.000026 ) -0.014306 0.028598 -0.014274 ( 0.000032 0.000041 0.000023 ) 0.007146 -0.014274 0.021409 ( 0.000026 0.000023 0.000026 ) unit cell: 5.913(6) 5.925(7) 5.935(5) 60.02(11) 90.02(8) 60.06(12) V = 147.2(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.070341 0.031270 0.088314 ( 0.000136 0.000101 0.000075 ) -0.068707 -0.065418 -0.010667 ( 0.000125 0.000093 0.000069 ) 0.108677 -0.152520 0.116088 ( 0.000164 0.000121 0.000090 ) M - matrix: 0.021479 -0.014280 0.007137 ( 0.000044 0.000031 0.000026 ) -0.014280 0.028520 -0.014246 ( 0.000031 0.000039 0.000022 ) 0.007137 -0.014246 0.021389 ( 0.000026 0.000022 0.000025 ) UB fit with 263 obs out of 275 (total:275,skipped:0) (95.64%) unit cell: 5.926(6) 5.936(6) 5.937(5) 60.03(10) 90.01(8) 60.02(11) V = 147.8(2) UB fit with 263 obs out of 275 (total:275,skipped:0) (95.64%) UB - matrix: -0.070341 0.031270 0.088314 ( 0.000136 0.000101 0.000075 ) -0.068707 -0.065418 -0.010667 ( 0.000125 0.000093 0.000069 ) 0.108677 -0.152520 0.116088 ( 0.000164 0.000121 0.000090 ) M - matrix: 0.021479 -0.014280 0.007137 ( 0.000044 0.000031 0.000026 ) -0.014280 0.028520 -0.014246 ( 0.000031 0.000039 0.000022 ) 0.007137 -0.014246 0.021389 ( 0.000026 0.000022 0.000025 ) unit cell: 5.926(6) 5.936(6) 5.937(5) 60.03(10) 90.01(8) 60.02(11) V = 147.8(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.070336 0.031288 0.088319 ( 0.000134 0.000099 0.000073 ) -0.068726 -0.065419 -0.010666 ( 0.000123 0.000091 0.000068 ) 0.108693 -0.152523 0.116087 ( 0.000160 0.000119 0.000088 ) M - matrix: 0.021484 -0.014283 0.007139 ( 0.000043 0.000030 0.000025 ) -0.014283 0.028522 -0.014245 ( 0.000030 0.000039 0.000022 ) 0.007139 -0.014245 0.021390 ( 0.000025 0.000022 0.000024 ) UB fit with 263 obs out of 275 (total:275,skipped:0) (95.64%) unit cell: 5.925(6) 5.935(6) 5.937(5) 60.04(10) 90.02(8) 60.02(11) V = 147.7(2) 275 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Run 2 Omega scan: (-103.000 - -53.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070336 0.031288 0.088319 ( 0.000134 0.000099 0.000073 ) -0.068726 -0.065419 -0.010666 ( 0.000123 0.000091 0.000068 ) 0.108693 -0.152523 0.116087 ( 0.000160 0.000119 0.000088 ) M - matrix: 0.021484 -0.014283 0.007139 ( 0.000043 0.000030 0.000025 ) -0.014283 0.028522 -0.014245 ( 0.000030 0.000039 0.000022 ) 0.007139 -0.014245 0.021390 ( 0.000025 0.000022 0.000024 ) UB fit with 263 obs out of 275 (total:275,skipped:0) (95.64%) unit cell: 5.925(6) 5.935(6) 5.937(5) 60.04(10) 90.02(8) 60.02(11) V = 147.7(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 263 obs out of 275 (total:275,skipped:0) (95.64%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb 3 of 208 peaks identified as outliers and rejected 205 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 205 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 205 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.28 | 21 | 0.990 ( 0.109) | 1.199 ( 0.511) | 1.199 ( 0.983) | 1.28- 1.09 | 21 | 1.042 ( 0.073) | 1.132 ( 0.119) | 0.997 ( 0.331) | 1.09- 0.94 | 21 | 1.006 ( 0.089) | 1.063 ( 0.153) | 1.075 ( 0.483) | 0.94- 0.84 | 21 | 0.997 ( 0.086) | 1.057 ( 0.141) | 1.061 ( 0.427) | 0.84- 0.78 | 21 | 1.002 ( 0.083) | 1.068 ( 0.147) | 0.981 ( 0.226) | 0.78- 0.73 | 21 | 0.994 ( 0.047) | 1.037 ( 0.159) | 1.062 ( 0.361) | 0.73- 0.69 | 21 | 0.962 ( 0.050) | 0.973 ( 0.214) | 1.282 ( 0.634) | 0.69- 0.65 | 21 | 0.964 ( 0.036) | 0.914 ( 0.110) | 1.135 ( 0.378) | 0.65- 0.63 | 21 | 0.922 ( 0.036) | 0.862 ( 0.049) | 1.366 ( 0.482) | 0.62- 0.59 | 16 | 0.887 ( 0.031) | 0.843 ( 0.077) | 1.122 ( 0.363) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 205 | 0.979 ( 0.081) | 1.019 ( 0.236) | 1.128 ( 0.525) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 205 obs out of 205 (total:205,skipped:0) (100.00%) UB - matrix: -0.070241 0.031036 0.088710 ( 0.000065 0.000048 0.000039 ) -0.068202 -0.065900 -0.010344 ( 0.000061 0.000045 0.000036 ) 0.109053 -0.152582 0.116285 ( 0.000057 0.000042 0.000034 ) M - matrix: 0.021478 -0.014325 0.007156 ( 0.000017 0.000012 0.000010 ) -0.014325 0.028587 -0.014308 ( 0.000012 0.000014 0.000009 ) 0.007156 -0.014308 0.021499 ( 0.000010 0.000009 0.000011 ) unit cell: 5.932(3) 5.936(3) 5.924(2) 60.00(5) 89.94(4) 59.92(5) V = 147.40(11) OTKP changes: 205 1 1 1 OTKP changes: 205 1 1 1 OTKP changes: 205 1 1 1 UB - matrix: -0.070439 0.031219 0.088607 ( 0.000063 0.000047 0.000038 ) -0.068478 -0.065877 -0.010384 ( 0.000053 0.000039 0.000032 ) 0.109047 -0.152786 0.116310 ( 0.000054 0.000039 0.000032 ) M - matrix: 0.021542 -0.014349 0.007153 ( 0.000016 0.000011 0.000010 ) -0.014349 0.028658 -0.014320 ( 0.000011 0.000013 0.000008 ) 0.007153 -0.014320 0.021487 ( 0.000010 0.000008 0.000010 ) UB fit with 205 obs out of 205 (total:205,skipped:0) (100.00%) unit cell: 5.920(3) 5.927(3) 5.925(2) 59.99(4) 89.93(3) 59.96(5) V = 146.95(9) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -53.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 426 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070439 0.031219 0.088607 ( 0.000063 0.000047 0.000038 ) -0.068478 -0.065877 -0.010384 ( 0.000053 0.000039 0.000032 ) 0.109047 -0.152786 0.116310 ( 0.000054 0.000039 0.000032 ) M - matrix: 0.021542 -0.014349 0.007153 ( 0.000016 0.000011 0.000010 ) -0.014349 0.028658 -0.014320 ( 0.000011 0.000013 0.000008 ) 0.007153 -0.014320 0.021487 ( 0.000010 0.000008 0.000010 ) UB fit with 205 obs out of 205 (total:205,skipped:0) (100.00%) unit cell: 5.920(3) 5.927(3) 5.925(2) 59.99(4) 89.93(3) 59.96(5) V = 146.95(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 205 obs out of 205 (total:205,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb 2 of 204 peaks identified as outliers and rejected 202 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 202 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 202 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.36 | 20 | 0.997 ( 0.136) | 1.321 ( 0.726) | 1.287 ( 1.075) | 1.32- 1.09 | 20 | 1.038 ( 0.074) | 1.102 ( 0.112) | 1.039 ( 0.376) | 1.09- 0.97 | 20 | 1.012 ( 0.092) | 1.076 ( 0.127) | 1.053 ( 0.484) | 0.96- 0.85 | 20 | 0.985 ( 0.088) | 1.033 ( 0.152) | 1.041 ( 0.346) | 0.85- 0.81 | 20 | 1.019 ( 0.081) | 1.082 ( 0.149) | 0.986 ( 0.200) | 0.81- 0.73 | 20 | 0.985 ( 0.053) | 1.042 ( 0.151) | 1.007 ( 0.300) | 0.73- 0.70 | 20 | 0.967 ( 0.061) | 0.937 ( 0.135) | 1.320 ( 0.672) | 0.70- 0.67 | 20 | 0.967 ( 0.032) | 0.915 ( 0.071) | 1.198 ( 0.444) | 0.66- 0.63 | 20 | 0.932 ( 0.035) | 0.876 ( 0.083) | 1.182 ( 0.418) | 0.63- 0.59 | 22 | 0.895 ( 0.038) | 0.846 ( 0.074) | 1.224 ( 0.437) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 202 | 0.979 ( 0.086) | 1.021 ( 0.288) | 1.134 ( 0.540) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.5 | 64 | 1.120 ( 0.055) | 1.255 ( 0.449) | 1.215 ( 0.603) | 13.7-19.7 | 64 | 1.112 ( 0.063) | 1.144 ( 0.201) | 1.282 ( 0.564) | 19.8-23.8 | 64 | 1.098 ( 0.083) | 1.163 ( 0.323) | 1.271 ( 0.623) | 23.8-28.1 | 64 | 1.067 ( 0.093) | 1.148 ( 0.435) | 1.286 ( 0.556) | 28.1-31.2 | 65 | 1.036 ( 0.094) | 0.980 ( 0.105) | 1.251 ( 0.454) | 31.3-34.5 | 64 | 1.025 ( 0.100) | 0.935 ( 0.112) | 1.247 ( 0.516) | 34.6-37.2 | 64 | 0.997 ( 0.089) | 0.891 ( 0.094) | 1.293 ( 0.522) | 37.2-39.7 | 64 | 0.982 ( 0.114) | 0.912 ( 0.213) | 1.276 ( 0.630) | 39.7-42.8 | 64 | 0.963 ( 0.103) | 0.849 ( 0.090) | 1.170 ( 0.479) | 42.8-49.8 | 66 | 0.966 ( 0.100) | 0.829 ( 0.080) | 1.158 ( 0.482) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 643 | 1.036 ( 0.107) | 1.010 ( 0.289) | 1.245 ( 0.548) | Fitted profile normalization line parameters e1 dimension: a=-0.0040 b=1.14 e2 dimension: a=-0.0101 b=1.28 e3 dimension: a=0.0029 b=0.98 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5033 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 8356951 lp-corr: 2433167 PROFFITPEAK - Finished at Tue Mar 27 13:44:43 2018 PROFFITMAIN - Started at Tue Mar 27 13:44:43 2018 OTKP changes: 643 1 2 2 OTKP changes: 643 1 2 2 UB - matrix: -0.070332 0.031078 0.088792 ( 0.000026 0.000022 0.000015 ) -0.068350 -0.066037 -0.010668 ( 0.000026 0.000022 0.000015 ) 0.109328 -0.153236 0.116383 ( 0.000023 0.000019 0.000013 ) M - matrix: 0.021571 -0.014425 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014425 0.028808 -0.014370 ( 0.000005 0.000007 0.000004 ) 0.007208 -0.014370 0.021543 ( 0.000004 0.000004 0.000004 ) UB fit with 643 obs out of 643 (total:643,skipped:0) (100.00%) unit cell: 5.9216(13) 5.9118(13) 5.9160(10) 60.08(2) 90.050(16) 59.93(2) V = 146.40(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070150 0.030737 0.088839 ( 0.000027 0.000027 0.000016 ) -0.068151 -0.066108 -0.010675 ( 0.000024 0.000024 0.000014 ) 0.109149 -0.153133 0.116141 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021479 -0.014365 0.007172 ( 0.000007 0.000005 0.000004 ) -0.014365 0.028765 -0.014349 ( 0.000005 0.000008 0.000004 ) 0.007172 -0.014349 0.021495 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9304(14) 5.9148(14) 5.9237(11) 60.04(2) 90.026(17) 59.97(2) V = 146.92(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070305 0.030887 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068361 -0.066109 -0.010680 ( 0.000023 0.000023 0.000013 ) 0.109305 -0.153230 0.116291 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021564 -0.014401 0.007199 ( 0.000007 0.000005 0.000004 ) -0.014401 0.028804 -0.014371 ( 0.000005 0.000008 0.000004 ) 0.007199 -0.014371 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9103(13) 5.9208(10) 60.04(2) 90.055(16) 59.99(2) V = 146.45(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.830) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070305 0.030887 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068361 -0.066109 -0.010680 ( 0.000023 0.000023 0.000013 ) 0.109305 -0.153230 0.116291 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021564 -0.014401 0.007199 ( 0.000007 0.000005 0.000004 ) -0.014401 0.028804 -0.014371 ( 0.000005 0.000008 0.000004 ) 0.007199 -0.014371 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9103(13) 5.9208(10) 60.04(2) 90.055(16) 59.99(2) V = 146.45(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070305 0.030887 0.088791 ( 0.000026 0.000026 0.000015 ) -0.068361 -0.066109 -0.010680 ( 0.000023 0.000023 0.000013 ) 0.109305 -0.153230 0.116291 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021564 -0.014401 0.007199 ( 0.000007 0.000005 0.000004 ) -0.014401 0.028804 -0.014371 ( 0.000005 0.000008 0.000004 ) 0.007199 -0.014371 0.021521 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9103(13) 5.9208(10) 60.04(2) 90.055(16) 59.99(2) V = 146.45(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) UB - matrix: -0.070546 0.031310 0.088590 ( 0.000064 0.000047 0.000038 ) -0.068652 -0.065871 -0.010382 ( 0.000071 0.000052 0.000042 ) 0.109076 -0.152894 0.116315 ( 0.000058 0.000043 0.000035 ) M - matrix: 0.021587 -0.014364 0.007150 ( 0.000018 0.000012 0.000010 ) -0.014364 0.028696 -0.014326 ( 0.000012 0.000015 0.000009 ) 0.007150 -0.014326 0.021485 ( 0.000010 0.000009 0.000011 ) unit cell: 5.911(3) 5.921(3) 5.925(2) 59.98(5) 89.92(4) 59.97(6) V = 146.65(11) OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 OTKP changes: 202 1 1 1 UB - matrix: -0.070517 0.031297 0.088821 ( 0.000064 0.000047 0.000038 ) -0.068761 -0.065844 -0.010383 ( 0.000067 0.000049 0.000040 ) 0.109222 -0.153126 0.116527 ( 0.000057 0.000042 0.000034 ) M - matrix: 0.021630 -0.014404 0.007178 ( 0.000018 0.000012 0.000010 ) -0.014404 0.028762 -0.014380 ( 0.000012 0.000015 0.000009 ) 0.007178 -0.014380 0.021576 ( 0.000010 0.000009 0.000010 ) UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) unit cell: 5.907(3) 5.917(3) 5.914(2) 59.97(5) 89.91(4) 59.95(6) V = 146.11(11) Run 2 Omega scan: (-103.000 - -53.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.830) HKL list info: 415 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070517 0.031297 0.088821 ( 0.000064 0.000047 0.000038 ) -0.068761 -0.065844 -0.010383 ( 0.000067 0.000049 0.000040 ) 0.109222 -0.153126 0.116527 ( 0.000057 0.000042 0.000034 ) M - matrix: 0.021630 -0.014404 0.007178 ( 0.000018 0.000012 0.000010 ) -0.014404 0.028762 -0.014380 ( 0.000012 0.000015 0.000009 ) 0.007178 -0.014380 0.021576 ( 0.000010 0.000009 0.000010 ) UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) unit cell: 5.907(3) 5.917(3) 5.914(2) 59.97(5) 89.91(4) 59.95(6) V = 146.11(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070517 0.031297 0.088821 ( 0.000064 0.000047 0.000038 ) -0.068761 -0.065844 -0.010383 ( 0.000067 0.000049 0.000040 ) 0.109222 -0.153126 0.116527 ( 0.000057 0.000042 0.000034 ) M - matrix: 0.021630 -0.014404 0.007178 ( 0.000018 0.000012 0.000010 ) -0.014404 0.028762 -0.014380 ( 0.000012 0.000015 0.000009 ) 0.007178 -0.014380 0.021576 ( 0.000010 0.000009 0.000010 ) UB fit with 202 obs out of 202 (total:202,skipped:0) (100.00%) unit cell: 5.907(3) 5.917(3) 5.914(2) 59.97(5) 89.91(4) 59.95(6) V = 146.11(11) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070292 0.031070 0.088787 ( 0.000027 0.000023 0.000015 ) -0.068373 -0.066011 -0.010654 ( 0.000026 0.000022 0.000015 ) 0.109329 -0.153153 0.116316 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.021569 -0.014415 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028779 -0.014352 ( 0.000005 0.000007 0.000004 ) 0.007204 -0.014352 0.021526 ( 0.000004 0.000004 0.000004 ) UB fit with 643 obs out of 643 (total:643,skipped:0) (100.00%) unit cell: 5.9214(13) 5.9134(13) 5.9173(10) 60.10(2) 90.062(16) 59.93(2) V = 146.50(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 42 reflections under beam stop or inside a detector rejection region 8 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof 901 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:44:45 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.830) Run 2 Omega scan: (-103.000 - -53.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.830) PROFFIT INFO: signal sum: min=271.0000 max=20158892.0000 PROFFIT INFO: signal sum lp corr: min=628.9998 max=2937498.1278 PROFFIT INFO: background sum: min=1069.0000 max=9015.0000 PROFFIT INFO: background sum sig2: min=597.0000 max=6230.0000 PROFFIT INFO: num of signal pixels: min=59 max=512 PROFFIT INFO: Inet: min=1006.3997 max=4699997.5000 PROFFIT INFO: sig(Inet): min=104.4462 max=47423.6055 PROFFIT INFO: Inet/sig(Inet): min=1.09 max=229.33 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 4 26 80 187 207 340 585 816 901 Percent 0.0 0.0 0.4 2.9 8.9 20.8 23.0 37.7 64.9 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 901 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 901 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4699998- 1314239 90 2068229.74 128.51 100.00 1286285- 756066 90 982456.80 109.25 100.00 750650- 295465 90 484688.68 95.29 100.00 292723- 183552 90 225552.03 72.00 100.00 183330- 144397 90 166817.39 54.35 100.00 144043- 108834 90 122128.27 37.42 100.00 108645- 80478 90 93068.21 30.67 100.00 80402- 5957 90 43138.92 19.63 100.00 5929- 3411 90 4447.77 5.64 97.78 3405- 1006 91 2656.98 4.41 73.63 ------------------------------------------------------------------------------------ 4699998- 1006 901 418856.04 55.66 97.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 90 754918.62 83.10 100.00 1.28- 1.03 90 570186.86 67.74 97.78 1.03- 0.89 90 583820.02 66.40 98.89 0.89- 0.78 90 410988.41 56.41 96.67 0.78- 0.72 90 400567.45 62.07 98.89 0.72- 0.65 90 392762.16 55.84 98.89 0.65- 0.60 90 286822.42 43.19 94.44 0.60- 0.55 90 298604.75 46.09 94.44 0.55- 0.50 90 264722.96 40.12 94.44 0.50- 0.40 91 227295.15 35.87 96.70 ------------------------------------------------------------------------------------ 5.26- 0.40 901 418856.04 55.66 97.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:44:45 2018 Sorting 901 observations 191 unique observations with > 7.00 F2/sig(F2) 901 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 49 159 Total number of frames 159 Maximum number of 191 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 901 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 49 159 Total number of frames 159 723 observations > 7.00 F2/sig(F2) 723 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 48 158 Total number of frames 158 Frame #58 of 158 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 3.6 (Out of 723 removed 92 = 631, unique = 173) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 631 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 48 158 Total number of frames 158 Frame #23 of 158 skipped from refinement Frame #58 of 158 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 173 unique data precomputed (should be 173) 173 unique data with 631 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 3.6 (Out of 631 removed 0 = 631, unique = 173) 173 unique data precomputed (should be 173) 173 unique data with 631 observations RMS deviation of equivalent data = 0.68033 Rint = 0.64071 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.61555, wR= 3.96498 Trying model 1 (ne=2, no=0)... Results: Rint= 0.78174, wR= 1.89488, Acormin=-0.215, Acormax=1.461, Acor_av=0.493 F test: Probability=0.000, F= 0.613 Trying model 2 (ne=2, no=1)... Results: Rint= 0.83501, wR= 1.89882, Acormin=-0.598, Acormax=1.388, Acor_av=0.267 F test: Probability=0.000, F= 0.534 Trying model 3 (ne=4, no=0)... Results: Rint= 0.89313, wR= 1.95489, Acormin=-0.368, Acormax=1.551, Acor_av=0.264 F test: Probability=0.000, F= 0.460 Trying model 4 (ne=4, no=1)... Results: Rint= 0.87440, wR= 1.32433, Acormin=-1.259, Acormax=1.274, Acor_av=0.150 F test: Probability=0.000, F= 0.477 Trying model 5 (ne=4, no=3)... Results: Rint= 0.92747, wR= 3.15225, Acormin=-0.514, Acormax=0.892, Acor_av=0.029 F test: Probability=0.000, F= 0.417 Trying model 6 (ne=6, no=0)... Results: Rint= 0.93738, wR= 2.38932, Acormin=-1.045, Acormax=1.712, Acor_av=0.159 F test: Probability=0.000, F= 0.406 Trying model 7 (ne=6, no=1)... Results: Rint= 0.90086, wR= 1.51716, Acormin=-1.743, Acormax=0.979, Acor_av=0.078 F test: Probability=0.000, F= 0.436 Trying model 8 (ne=6, no=3)... Results: Rint= 0.90266, wR= 3.02705, Acormin=-0.541, Acormax=0.760, Acor_av=0.023 F test: Probability=0.000, F= 0.427 Trying model 9 (ne=6, no=5)... Results: Rint= 0.96924, wR= 3.28115, Acormin=-0.162, Acormax=0.359, Acor_av=0.005 F test: Probability=0.000, F= 0.361 Trying model 10 (ne=8, no=0)... Results: Rint= 0.91913, wR= 2.88369, Acormin=-0.825, Acormax=1.066, Acor_av=-0.004 F test: Probability=0.000, F= 0.405 Trying model 11 (ne=8, no=1)... Results: Rint= 0.85859, wR= 2.30610, Acormin=-0.604, Acormax=0.329, Acor_av=0.009 F test: Probability=0.000, F= 0.461 Trying model 12 (ne=8, no=3)... Results: Rint= 0.91744, wR= 2.05304, Acormin=-0.041, Acormax=0.051, Acor_av=0.001 F test: Probability=0.000, F= 0.397 Trying model 13 (ne=8, no=5)... Results: Rint= 0.90632, wR= 2.47335, Acormin=-0.042, Acormax=0.054, Acor_av=0.001 F test: Probability=0.000, F= 0.395 Trying model 14 (ne=8, no=7)... Results: Rint= 0.90617, wR= 2.07877, Acormin=-0.019, Acormax=0.028, Acor_av=0.001 F test: Probability=0.000, F= 0.380 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.78300 There are 156 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 160 pars with 12880 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.68033 Using Levenberg-Marquardt: 0.00010 New wR= 0.65364 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.64071 with corrections 0.60441 Rint for all data: 0.78300 with corrections 0.75728 2 observations identified as outliers and rejected Cycle 2 wR= 0.65024 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63909 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.62822 with corrections 0.58988 Rint for all data: 0.78300 with corrections 0.75601 2 observations identified as outliers and rejected Cycle 3 wR= 0.63463 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.62840 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.61555 with corrections 0.58098 Rint for all data: 0.78300 with corrections 0.75726 2 observations identified as outliers and rejected Cycle 4 wR= 0.60479 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60047 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60507 with corrections 0.57411 Rint for all data: 0.78300 with corrections 0.76038 1 observations identified as outliers and rejected Cycle 5 wR= 0.59506 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59278 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60314 with corrections 0.57563 Rint for all data: 0.78300 with corrections 0.76258 1 observations identified as outliers and rejected Final wR= 0.59278 Final frame scales: Min= 0.7925 Max= 9.6110 Final absorption correction factors: Amin= 0.3745 Amax= 1.8867 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 156 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 160 pars with 12880 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.77603 Using Levenberg-Marquardt: 0.00010 New wR= 0.61975 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60211 with corrections 0.86254 Rint for all data: 0.78300 with corrections 0.97184 1 observations identified as outliers and rejected Cycle 2 wR= 0.61869 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59451 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60017 with corrections 0.65597 Rint for all data: 0.78300 with corrections 0.81583 0 observations identified as outliers and rejected Cycle 3 wR= 0.59451 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58910 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60017 with corrections 0.62567 Rint for all data: 0.78300 with corrections 0.79563 0 observations identified as outliers and rejected Cycle 4 wR= 0.58910 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58685 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60017 with corrections 0.61664 Rint for all data: 0.78300 with corrections 0.78966 0 observations identified as outliers and rejected Cycle 5 wR= 0.58685 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.58924 Using Levenberg-Marquardt: 1.00000 New wR= 0.58617 There are 3 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60017 with corrections 0.61478 Rint for all data: 0.78300 with corrections 0.78840 0 observations identified as outliers and rejected Final wR= 0.58617 Final frame scales: Min= 0.6882 Max= 9.5809 Final absorption correction factors: Amin= 0.1498 Amax= 2.2184 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 153 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 157 pars with 12403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.78905 Using Levenberg-Marquardt: 0.00010 New wR= 0.65321 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60017 with corrections 1.00152 Rint for all data: 0.78300 with corrections 1.09532 0 observations identified as outliers and rejected Cycle 2 wR= 0.64777 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61183 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60017 with corrections 0.98926 Rint for all data: 0.78300 with corrections 1.09725 0 observations identified as outliers and rejected Cycle 3 wR= 0.61231 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59925 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60017 with corrections 0.73884 Rint for all data: 0.78300 with corrections 0.89673 0 observations identified as outliers and rejected Cycle 4 wR= 0.59951 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59541 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60017 with corrections 0.64441 Rint for all data: 0.78300 with corrections 0.81203 0 observations identified as outliers and rejected Cycle 5 wR= 0.59537 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59295 There are 5 clusters with unrefined scales (size 1-2) Rint for refined data: 0.60017 with corrections 0.63085 Rint for all data: 0.78300 with corrections 0.80076 0 observations identified as outliers and rejected Final wR= 0.59295 Final frame scales: Min= 0.5369 Max= 4.7078 Final absorption correction factors: Amin= 0.0591 Amax= 2.1813 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=804.1818 max=6084029.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=144.4752 max=84038.7969 PROFFIT INFO: 6 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/109 895 reflections read from tmp file 757 reflections are rejected (604 as outliers, 153 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 51 8 3 Initial Chi^2= 0.94174 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.03272 Current error model SIG(F2)^2 = 261.10*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 269.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 269.64*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6084029- 1193430 89 2072699.79 85.52 100.00 1153219- 612863 89 843216.87 51.38 100.00 606272- 276897 89 413114.96 37.22 100.00 276534- 193972 89 230767.14 31.82 100.00 191364- 130154 89 154884.48 22.74 100.00 129772- 94470 89 109661.10 17.18 100.00 93009- 58540 89 76877.73 14.42 100.00 58533- 6306 89 34156.26 9.45 89.89 6247- 3163 89 4283.08 3.39 49.44 3149- 804 94 2129.59 2.92 31.91 ------------------------------------------------------------------------------------ 6084029- 804 895 391988.88 27.47 86.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 89 691094.93 59.31 97.75 1.28- 1.03 89 574495.91 38.46 95.51 1.03- 0.89 89 645390.64 35.11 91.01 0.89- 0.78 89 372069.48 24.14 80.90 0.78- 0.72 89 439316.75 26.61 92.13 0.72- 0.65 89 354917.30 23.81 86.52 0.65- 0.60 89 242996.83 16.74 77.53 0.60- 0.55 89 283271.65 19.71 82.02 0.55- 0.51 89 197729.91 16.98 83.15 0.51- 0.40 94 133147.10 14.52 81.91 ------------------------------------------------------------------------------------ 5.26- 0.40 895 391988.88 27.47 86.82 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 89 691094.93 59.31 97.75 5.26- 1.03 178 632795.42 48.88 96.63 5.26- 0.89 267 636993.83 44.29 94.76 5.26- 0.78 356 570762.74 39.26 91.29 5.26- 0.72 445 544473.54 36.73 91.46 5.26- 0.65 534 512880.83 34.57 90.64 5.26- 0.60 623 474325.98 32.03 88.76 5.26- 0.55 712 450444.18 30.49 87.92 5.26- 0.51 801 422364.82 28.98 87.39 5.26- 0.40 895 391988.88 27.47 86.82 ------------------------------------------------------------------------------------ 5.26- 0.40 895 391988.88 27.47 86.82 Scale applied to data: s=0.164365 (maximum obs:6084029.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.797; Rsigma 0.024: data 895 -> merged 291 With outlier rejection... Rint 0.574; Rsigma 0.027: data 734 -> merged 291 Rejected total: 161, method kkm 160, method Blessing 1 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404318, 5.271657 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 2.93 100.00 44 1.46 - 1.12 15 15 5.20 100.00 78 1.08 - 0.96 15 15 4.33 100.00 65 0.96 - 0.86 15 15 4.47 100.00 67 0.86 - 0.79 15 15 3.27 100.00 49 0.79 - 0.73 15 15 3.60 100.00 54 0.73 - 0.69 15 15 2.53 100.00 38 0.69 - 0.65 15 15 2.73 100.00 41 0.65 - 0.63 15 15 2.07 100.00 31 0.63 - 0.60 21 21 2.33 100.00 49 --------------------------------------------------------------- 5.92 - 0.60 156 156 3.31 100.00 516 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:44:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921397 5.913399 5.917308 60.0990 90.0615 59.9324 734 Reflections read from file xs1714a.hkl; mean (I/sigma) = 24.74 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 366 401 355 379 561 494 502 734 N (int>3sigma) = 0 315 401 304 325 510 428 434 635 Mean intensity = 0.0 44.7 26.6 44.4 50.3 38.1 50.5 50.1 48.4 Mean int/sigma = 0.0 23.8 22.5 24.0 24.9 23.4 25.6 25.0 24.7 Lattice type: P chosen Volume: 146.50 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.911 5.913 5.916 90.03 119.96 119.90 Niggli form: a.a = 34.944 b.b = 34.968 c.c = 34.997 b.c = -0.019 a.c = -17.463 a.b = -17.425 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.161 CUBIC F-lattice R(int) = 0.271 [ 584] Vol = 586.0 Cell: 8.367 8.376 8.362 90.12 89.98 89.96 Volume: 586.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.146 RHOMBOHEDRAL R-lattice R(int) = 0.268 [ 369] Vol = 439.5 Cell: 5.921 5.913 14.503 89.96 90.09 120.07 Volume: 439.50 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.146 RHOMBOHEDRAL R-lattice R(int) = 0.306 [ 105] Vol = 439.5 Trigonal Cell: 5.921 5.913 14.503 89.96 90.09 120.07 Volume: 439.50 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.069 TETRAGONAL I-lattice R(int) = 0.220 [ 383] Vol = 293.0 Cell: 5.917 5.921 8.362 89.93 89.90 89.94 Volume: 293.00 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.146 TETRAGONAL I-lattice R(int) = 0.220 [ 383] Vol = 293.0 Cell: 5.921 5.917 8.362 90.10 90.07 89.94 Volume: 293.00 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.078 ORTHORHOMBIC I-lattice R(int) = 0.224 [ 400] Vol = 293.0 Cell: 5.921 5.917 8.362 89.90 89.93 89.94 Volume: 293.00 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.242 [ 359] Vol = 293.0 Cell: 5.911 8.367 5.924 90.01 89.91 90.04 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.225 [ 220] Vol = 293.0 Cell: 5.917 5.921 8.362 90.07 90.10 89.94 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.066 MONOCLINIC I-lattice R(int) = 0.226 [ 229] Vol = 293.0 Cell: 5.911 5.924 8.367 89.99 90.04 90.09 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.043 MONOCLINIC I-lattice R(int) = 0.226 [ 194] Vol = 293.0 Cell: 5.911 8.367 5.924 90.01 90.09 89.96 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.127 MONOCLINIC C-lattice R(int) = 0.261 [ 251] Vol = 293.0 Cell: 10.249 5.913 5.916 90.03 125.19 89.89 Volume: 293.00 Matrix:-2.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.223 [ 43] Vol = 146.5 Cell: 5.911 5.913 5.916 90.03 119.96 119.90 Volume: 146.50 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 401 0 503 487 734 N (int>3sigma) = 0 0 0 0 401 0 432 426 635 Mean intensity = 0.0 0.0 0.0 0.0 26.6 0.0 49.4 48.8 48.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.5 0.0 25.0 25.0 24.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.021 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 57 165 N I>3s 9 9 39 165 0.7 0.7 0.8 27.8 7.3 7.3 4.0 27.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.271 546 Fd-3m 1 1 227 C N N N N 37 2284 0.284 583 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366735 8.375721 8.362291 90.1244 89.9767 89.9604 ZERR 1.00 0.000464 0.002834 0.006329 0.0037 0.0207 0.0030 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3041435- 760538 113 88 29 3.0 967420.91 54.49 0.515 0.398 736946- 552467 118 103 29 3.6 518892.40 36.53 0.739 0.590 537514- 383676 105 78 29 2.7 319027.05 24.05 0.627 0.486 383201- 253929 115 87 29 3.0 198223.61 21.50 0.502 0.468 249615- 173074 105 86 29 3.0 162329.03 25.72 0.579 0.640 172669- 112743 110 90 29 3.1 121418.57 18.48 0.381 0.326 112691- 76606 73 63 29 2.2 89256.65 13.59 0.463 0.307 76578- 51664 53 46 29 1.6 65513.79 11.95 0.253 0.257 51553- 6693 59 49 29 1.7 38300.51 8.62 0.390 0.391 5689- 992 44 44 30 1.5 3435.22 3.47 0.161 0.183 ------------------------------------------------------------------------------------------- 3041435- 992 895 734 291 2.5 294633.74 24.74 0.574 0.460 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 135 111 29 3.8 489317.86 47.58 0.497 0.382 0.015 1.12-0.87 155 133 29 4.6 421660.90 29.60 0.834 0.782 0.022 0.86-0.75 130 102 29 3.5 265291.69 22.35 0.479 0.350 0.032 0.74-0.67 106 78 29 2.7 332638.03 23.83 0.554 0.509 0.028 0.66-0.61 87 72 32 2.3 128473.37 13.03 0.509 0.435 0.052 0.61-0.57 80 64 29 2.2 306782.64 21.26 0.352 0.317 0.033 0.56-0.53 66 53 30 1.8 152384.97 14.94 0.295 0.295 0.047 0.53-0.49 65 54 30 1.8 122205.66 12.58 0.423 0.465 0.049 0.49-0.46 43 39 29 1.3 154578.89 16.69 0.436 0.436 0.040 0.45-0.40 28 28 25 1.1 116864.57 13.69 0.858 0.858 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 895 734 291 2.5 294633.74 24.74 0.574 0.460 0.027 inf-0.60 638 516 156 3.3 348791.81 28.68 0.607 0.489 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 111 29 29 100.0 3.8 489317.86 101.42 0.497 0.008 1.12-0.87 133 29 29 100.0 4.6 421660.90 78.63 0.834 0.014 0.86-0.75 102 29 29 100.0 3.5 265291.69 44.58 0.479 0.018 0.74-0.67 78 29 29 100.0 2.7 332638.03 46.52 0.554 0.020 0.66-0.61 72 32 32 100.0 2.3 128473.37 21.63 0.509 0.038 0.61-0.57 64 34 29 85.3 2.2 306782.64 33.98 0.352 0.023 0.56-0.53 53 33 30 90.9 1.8 152384.97 21.09 0.295 0.033 0.53-0.49 54 50 30 60.0 1.8 122205.66 17.49 0.423 0.046 0.49-0.46 39 66 29 43.9 1.3 154578.89 21.48 0.436 0.030 0.45-0.40 28 127 25 19.7 1.1 116864.57 15.26 0.858 0.044 -------------------------------------------------------------------------------------------- inf-0.40 734 462 291 63.0 2.5 294633.74 50.34 0.574 0.018 inf-0.60 516 156 156 100.0 3.3 348791.81 62.72 0.607 0.015 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 0.0 1.0 -1.0 2.0 -1.0 No constraint UB - matrix: -0.024783 0.079539 0.015535 ( 0.000011 0.000012 0.000012 ) 0.072519 0.028860 -0.033006 ( 0.000011 0.000011 0.000011 ) -0.036246 0.003493 -0.076577 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007187 -0.000005 -0.000003 ( 0.000002 0.000001 0.000001 ) -0.000005 0.007172 0.000016 ( 0.000001 0.000002 0.000001 ) -0.000003 0.000016 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024783 0.079539 0.015535 ( 0.000011 0.000012 0.000012 ) 0.072519 0.028860 -0.033006 ( 0.000011 0.000011 0.000011 ) -0.036246 0.003493 -0.076577 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) unit cell: 8.3667(11) 8.3757(11) 8.3623(10) 90.124(10) 89.977(10) 89.960(11) V = 586.01(13) unit cell: 8.3682(3) 8.3682(3) 8.3682(3) 90.0 90.0 90.0 V = 586.01(4) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.830) Run 2 Omega scan: (-103.000 - -53.000,50 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.830) PROFFIT INFO: signal sum: min=271.0000 max=20158892.0000 PROFFIT INFO: signal sum lp corr: min=628.9998 max=2937498.1278 PROFFIT INFO: background sum: min=1069.0000 max=9015.0000 PROFFIT INFO: background sum sig2: min=597.0000 max=6230.0000 PROFFIT INFO: num of signal pixels: min=59 max=512 PROFFIT INFO: Inet: min=1006.3997 max=4699997.5000 PROFFIT INFO: sig(Inet): min=104.4462 max=47423.6055 PROFFIT INFO: Inet/sig(Inet): min=1.09 max=229.33 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 52 160 374 414 680 1170 1632 1802 Percent 0.0 0.0 0.4 2.9 8.9 20.8 23.0 37.7 64.9 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 901 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 901 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4699998- 1314239 90 2068229.74 128.51 100.00 1286285- 756066 90 982456.80 109.25 100.00 750650- 295465 90 484688.68 95.29 100.00 292723- 183552 90 225552.03 72.00 100.00 183330- 144397 90 166817.39 54.35 100.00 144043- 108834 90 122128.27 37.42 100.00 108645- 80478 90 93068.21 30.67 100.00 80402- 5957 90 43138.92 19.63 100.00 5929- 3411 90 4447.77 5.64 97.78 3405- 1006 91 2656.98 4.41 73.63 ------------------------------------------------------------------------------------ 4699998- 1006 901 418856.04 55.66 97.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 90 728817.29 81.55 100.00 1.39- 1.09 90 849416.59 73.90 100.00 1.09- 0.96 90 416863.61 69.15 100.00 0.96- 0.84 90 548934.45 74.54 97.78 0.84- 0.80 90 413899.01 62.64 100.00 0.80- 0.73 90 283241.40 45.90 100.00 0.73- 0.70 90 283166.84 41.66 86.67 0.69- 0.65 90 299284.61 46.20 98.89 0.65- 0.62 90 184521.98 31.37 91.11 0.62- 0.58 91 183034.81 29.98 96.70 ------------------------------------------------------------------------------------ 4.82- 0.58 901 418856.04 55.66 97.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:44:46 2018 Sorting 901 observations 80 unique observations with > 7.00 F2/sig(F2) 901 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 49 159 Total number of frames 159 Maximum number of 80 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 901 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 24 80 Total number of frames 80 723 observations > 7.00 F2/sig(F2) 723 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 24 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 723 removed 6 = 717, unique = 84) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 717 observations in 2 runs Run # start # end # total # 1 0 54 55 2 0 24 80 Total number of frames 80 84 unique data precomputed (should be 84) 84 unique data with 717 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 717 removed 0 = 717, unique = 84) 84 unique data precomputed (should be 84) 84 unique data with 717 observations RMS deviation of equivalent data = 0.08962 Rint = 0.07211 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.06942, wR= 0.09452 Trying model 1 (ne=2, no=0)... Results: Rint= 0.04360, wR= 0.05775, Acormin=0.843, Acormax=1.205, Acor_av=0.992 F test: Probability=1.000, F= 2.515 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04218, wR= 0.05607, Acormin=0.843, Acormax=1.209, Acor_av=1.007 F test: Probability=0.780, F= 1.064 Trying model 3 (ne=4, no=0)... Results: Rint= 0.03311, wR= 0.04530, Acormin=0.779, Acormax=1.178, Acor_av=0.954 F test: Probability=1.000, F= 1.710 Trying model 4 (ne=4, no=1)... Results: Rint= 0.02917, wR= 0.03978, Acormin=0.708, Acormax=1.180, Acor_av=0.941 F test: Probability=0.999, F= 1.281 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02788, wR= 0.03584, Acormin=0.734, Acormax=1.202, Acor_av=0.924 F test: Probability=0.836, F= 1.082 Trying model 6 (ne=6, no=0)... Results: Rint= 0.02993, wR= 0.04079, Acormin=0.735, Acormax=1.188, Acor_av=0.946 F test: Probability=0.000, F= 0.935 Trying model 7 (ne=6, no=1)... Results: Rint= 0.02679, wR= 0.03699, Acormin=0.732, Acormax=1.160, Acor_av=0.941 F test: Probability=0.967, F= 1.161 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02329, wR= 0.03022, Acormin=0.749, Acormax=1.306, Acor_av=0.933 F test: Probability=0.999, F= 1.307 Trying model 9 (ne=6, no=5)... Results: Rint= 0.01803, wR= 0.02392, Acormin=0.771, Acormax=1.295, Acor_av=0.963 F test: Probability=1.000, F= 1.638 Trying model 10 (ne=8, no=0)... Results: Rint= 0.02633, wR= 0.03411, Acormin=0.742, Acormax=1.225, Acor_av=0.955 F test: Probability=0.000, F= 0.472 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02398, wR= 0.03106, Acormin=0.747, Acormax=1.172, Acor_av=0.933 F test: Probability=0.000, F= 0.567 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02045, wR= 0.02640, Acormin=0.769, Acormax=1.288, Acor_av=0.956 F test: Probability=0.000, F= 0.770 Trying model 13 (ne=8, no=5)... Results: Rint= 0.01680, wR= 0.02241, Acormin=0.768, Acormax=1.299, Acor_av=0.967 F test: Probability=0.910, F= 1.118 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01551, wR= 0.02093, Acormin=0.764, Acormax=1.311, Acor_av=0.970 F test: Probability=0.998, F= 1.277 Final absorption model (ne=8, no=7): Rint= 0.01551, Acormin=0.764, Acormax=1.311, Acor_av=0.970 Combined refinement in use Rint: 0.07229 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.08962 Using Levenberg-Marquardt: 0.00010 New wR= 0.01861 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07211 with corrections 0.01471 Rint for all data: 0.07229 with corrections 0.01496 1 observations identified as outliers and rejected Cycle 2 wR= 0.01843 Using Levenberg-Marquardt: 0.00001 New wR= 0.01786 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07215 with corrections 0.01433 Rint for all data: 0.07229 with corrections 0.01465 0 observations identified as outliers and rejected Cycle 3 wR= 0.01786 Using Levenberg-Marquardt: 0.00000 New wR= 0.01778 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07215 with corrections 0.01426 Rint for all data: 0.07229 with corrections 0.01458 1 observations identified as outliers and rejected Cycle 4 wR= 0.01786 Using Levenberg-Marquardt: 0.00000 New wR= 0.01783 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07137 with corrections 0.01422 Rint for all data: 0.07229 with corrections 0.01456 0 observations identified as outliers and rejected Cycle 5 wR= 0.01783 Using Levenberg-Marquardt: 0.00000 New wR= 0.01784 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07137 with corrections 0.01425 Rint for all data: 0.07229 with corrections 0.01458 Final wR= 0.01784 Final frame scales: Min= 0.9397 Max= 1.0917 Final absorption correction factors: Amin= 0.6867 Amax= 1.1609 PROFFIT INFO: Inet (after scale3 abspack): min=982.0807 max=4757574.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=124.7777 max=45942.6875 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/109 901 reflections read from tmp file 19 reflections are rejected (15 as outliers, 4 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 11 3 5 11 9 13 8 37 Initial Chi^2= 0.26210 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.14175 Current error model SIG(F2)^2 = 101.66*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 217.73*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 217.73*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4757575- 1228638 90 2064352.54 103.49 100.00 1227811- 740666 90 967985.51 48.75 100.00 739245- 315698 90 490685.67 48.73 100.00 295689- 187037 90 221615.48 32.79 100.00 186985- 149078 90 167691.90 23.62 100.00 148550- 105339 90 118832.16 16.77 100.00 105219- 81901 90 93529.39 14.27 100.00 80889- 5822 90 43684.16 9.55 98.89 5805- 3380 90 4392.35 3.63 71.11 3370- 982 91 2673.42 3.17 46.15 ------------------------------------------------------------------------------------ 4757575- 982 901 417083.80 30.45 91.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 90 735125.97 64.64 100.00 1.39- 1.09 90 854094.36 55.49 100.00 1.09- 0.96 90 417835.55 32.77 96.67 0.96- 0.84 90 539514.75 34.33 88.89 0.84- 0.80 90 411077.72 28.22 96.67 0.80- 0.73 90 280257.00 20.87 94.44 0.73- 0.70 90 279091.22 19.06 80.00 0.69- 0.65 90 293358.68 20.87 93.33 0.65- 0.62 90 183013.10 14.49 84.44 0.62- 0.58 91 180102.80 13.90 81.32 ------------------------------------------------------------------------------------ 4.82- 0.58 901 417083.80 30.45 91.56 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 90 735125.97 64.64 100.00 4.82- 1.09 180 794610.16 60.07 100.00 4.82- 0.96 270 669018.62 50.97 98.89 4.82- 0.84 360 636642.66 46.81 96.39 4.82- 0.80 450 591529.67 43.09 96.44 4.82- 0.73 540 539650.89 39.39 96.11 4.82- 0.70 630 502428.08 36.48 93.81 4.82- 0.65 720 476294.40 34.53 93.75 4.82- 0.62 810 443707.59 32.30 92.72 4.82- 0.58 901 417083.80 30.45 91.56 ------------------------------------------------------------------------------------ 4.82- 0.58 901 417083.80 30.45 91.56 Scale applied to data: s=0.210191 (maximum obs:4757574.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.015; Rsigma 0.021: data 901 -> merged 106 With outlier rejection... Rint 0.014; Rsigma 0.021: data 894 -> merged 106 Rejected total: 7, method kkm 6, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585894, 4.831402 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 9 10 4.56 90.00 41 1.61 - 1.21 10 10 8.10 100.00 81 1.17 - 1.01 10 10 10.20 100.00 102 0.99 - 0.89 10 10 10.40 100.00 104 0.88 - 0.81 10 10 10.40 100.00 104 0.81 - 0.74 10 10 8.50 100.00 85 0.73 - 0.71 10 10 10.00 100.00 100 0.70 - 0.66 10 10 8.50 100.00 85 0.66 - 0.64 10 10 7.30 100.00 73 0.63 - 0.60 10 10 7.40 100.00 74 --------------------------------------------------------------- 5.92 - 0.60 99 100 8.58 99.00 849 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:44:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.921397 5.913399 5.917308 60.0990 90.0615 59.9324 734 Reflections read from file xs1714a.hkl; mean (I/sigma) = 24.74 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 366 401 355 379 561 494 502 734 N (int>3sigma) = 0 315 401 304 325 510 428 434 635 Mean intensity = 0.0 44.7 26.6 44.4 50.3 38.1 50.5 50.1 48.4 Mean int/sigma = 0.0 23.8 22.5 24.0 24.9 23.4 25.6 25.0 24.7 Lattice type: P chosen Volume: 146.50 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.911 5.913 5.916 90.03 119.96 119.90 Niggli form: a.a = 34.944 b.b = 34.968 c.c = 34.997 b.c = -0.019 a.c = -17.463 a.b = -17.425 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.161 CUBIC F-lattice R(int) = 0.271 [ 584] Vol = 586.0 Cell: 8.367 8.376 8.362 90.12 89.98 89.96 Volume: 586.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.146 RHOMBOHEDRAL R-lattice R(int) = 0.268 [ 369] Vol = 439.5 Cell: 5.921 5.913 14.503 89.96 90.09 120.07 Volume: 439.50 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.146 RHOMBOHEDRAL R-lattice R(int) = 0.306 [ 105] Vol = 439.5 Trigonal Cell: 5.921 5.913 14.503 89.96 90.09 120.07 Volume: 439.50 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.069 TETRAGONAL I-lattice R(int) = 0.220 [ 383] Vol = 293.0 Cell: 5.917 5.921 8.362 89.93 89.90 89.94 Volume: 293.00 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.146 TETRAGONAL I-lattice R(int) = 0.220 [ 383] Vol = 293.0 Cell: 5.921 5.917 8.362 90.10 90.07 89.94 Volume: 293.00 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.078 ORTHORHOMBIC I-lattice R(int) = 0.224 [ 400] Vol = 293.0 Cell: 5.921 5.917 8.362 89.90 89.93 89.94 Volume: 293.00 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.056 ORTHORHOMBIC I-lattice R(int) = 0.242 [ 359] Vol = 293.0 Cell: 5.911 8.367 5.924 90.01 89.91 90.04 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.045 MONOCLINIC I-lattice R(int) = 0.225 [ 220] Vol = 293.0 Cell: 5.917 5.921 8.362 90.07 90.10 89.94 Volume: 293.00 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.066 MONOCLINIC I-lattice R(int) = 0.226 [ 229] Vol = 293.0 Cell: 5.911 5.924 8.367 89.99 90.04 90.09 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.043 MONOCLINIC I-lattice R(int) = 0.226 [ 194] Vol = 293.0 Cell: 5.911 8.367 5.924 90.01 90.09 89.96 Volume: 293.00 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.127 MONOCLINIC C-lattice R(int) = 0.261 [ 251] Vol = 293.0 Cell: 10.249 5.913 5.916 90.03 125.19 89.89 Volume: 293.00 Matrix:-2.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.223 [ 43] Vol = 146.5 Cell: 5.911 5.913 5.916 90.03 119.96 119.90 Volume: 146.50 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 401 0 503 487 734 N (int>3sigma) = 0 0 0 0 401 0 432 426 635 Mean intensity = 0.0 0.0 0.0 0.0 26.6 0.0 49.4 48.8 48.4 Mean int/sigma = 0.0 0.0 0.0 0.0 22.5 0.0 25.0 25.0 24.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.021 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 57 165 N I>3s 9 9 39 165 0.7 0.7 0.8 27.8 7.3 7.3 4.0 27.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.271 546 Fd-3m 1 1 227 C N N N N 37 2284 0.284 583 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366735 8.375721 8.362291 90.1244 89.9767 89.9604 ZERR 1.00 0.000464 0.002834 0.006329 0.0037 0.0207 0.0030 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4702313- 644318 199 196 26 7.5 1424846.67 70.81 0.011 0.013 606921- 145519 260 258 26 9.9 256822.08 34.24 0.017 0.018 128876- 65527 217 217 26 8.3 96901.50 14.21 0.029 0.035 43560- 2334 225 223 28 8.0 5982.08 4.25 0.093 0.117 ------------------------------------------------------------------------------------------- 4702313- 2334 901 894 106 8.4 411511.94 29.91 0.014 0.015 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 212 206 26 7.9 714644.05 54.76 0.014 0.015 0.012 1.01-0.78 256 256 26 9.8 443578.90 30.25 0.010 0.011 0.021 0.78-0.66 239 238 26 9.2 308699.79 21.16 0.014 0.016 0.030 0.66-0.59 194 194 28 6.9 173444.60 13.81 0.025 0.028 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 901 894 106 8.4 411511.94 29.91 0.014 0.015 0.021 inf-0.60 854 847 98 8.6 426447.87 30.86 0.013 0.015 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 206 27 26 96.3 7.9 714644.05 159.28 0.014 0.004 1.01-0.78 256 26 26 100.0 9.8 443578.90 100.39 0.010 0.007 0.78-0.66 238 26 26 100.0 9.2 308699.79 68.24 0.014 0.011 0.66-0.59 194 31 28 90.3 6.9 173444.60 40.67 0.025 0.019 -------------------------------------------------------------------------------------------- inf-0.59 894 110 106 96.4 8.4 411511.94 92.44 0.014 0.007 inf-0.60 847 99 98 99.0 8.6 426447.87 95.67 0.013 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:51:52 2018) ID: 2932; threads 39; handles 878; mem 518120.00 (1237820.00)kB; time: 1w 4d 22h 57m 22s MEMORY INFO: Memory PF:240.0, Ph:421.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.0,peak PF: 697.1, WS: 297.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:243.0, Ph:421.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.8,peak PF: 697.1, WS: 298.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:51:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000027 0.000023 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000026 0.000022 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000020 0.000013 ) 5.91502 ( 0.00132 ) 5.91640 ( 0.00133 ) 5.92265 ( 0.00101 ) 60.05206 ( 0.02098 ) 89.98756 ( 0.01620 ) 60.01743 ( 0.02343 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:51:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000027 0.000023 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000026 0.000022 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.021569 -0.014415 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028779 -0.014352 ( 0.000005 0.000007 0.000004 ) 0.007204 -0.014352 0.021526 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9150(13) 5.9164(13) 5.9227(10) 60.05(2) 89.988(16) 60.02(2) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb PROFFITPEAK info: 871 peaks in the peak location table UB fit with 387 obs out of 406 (total:406,skipped:0) (95.32%) UB - matrix: -0.070359 0.031298 0.088346 ( 0.000081 0.000059 0.000060 ) -0.068689 -0.065614 -0.010707 ( 0.000083 0.000060 0.000062 ) 0.108798 -0.152813 0.116145 ( 0.000102 0.000074 0.000075 ) M - matrix: 0.021506 -0.014321 0.007156 ( 0.000027 0.000019 0.000017 ) -0.014321 0.028637 -0.014281 ( 0.000019 0.000024 0.000016 ) 0.007156 -0.014281 0.021409 ( 0.000017 0.000016 0.000021 ) unit cell: 5.922(4) 5.923(4) 5.934(3) 60.06(7) 90.06(5) 60.03(7) V = 147.30(15) UB fit with 387 obs out of 406 (total:406,skipped:0) (95.32%) UB - matrix: -0.070359 0.031298 0.088346 ( 0.000081 0.000059 0.000060 ) -0.068689 -0.065614 -0.010707 ( 0.000083 0.000060 0.000062 ) 0.108798 -0.152813 0.116145 ( 0.000102 0.000074 0.000075 ) M - matrix: 0.021506 -0.014321 0.007156 ( 0.000027 0.000019 0.000017 ) -0.014321 0.028637 -0.014281 ( 0.000019 0.000024 0.000016 ) 0.007156 -0.014281 0.021409 ( 0.000017 0.000016 0.000021 ) unit cell: 5.922(4) 5.923(4) 5.934(3) 60.06(7) 90.06(5) 60.03(7) V = 147.30(15) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.070230 0.031164 0.088378 ( 0.000079 0.000057 0.000059 ) -0.068440 -0.065604 -0.010634 ( 0.000081 0.000059 0.000060 ) 0.108717 -0.152526 0.116094 ( 0.000099 0.000072 0.000074 ) M - matrix: 0.021436 -0.014281 0.007142 ( 0.000027 0.000019 0.000017 ) -0.014281 0.028539 -0.014256 ( 0.000019 0.000024 0.000016 ) 0.007142 -0.014256 0.021402 ( 0.000017 0.000016 0.000020 ) UB fit with 389 obs out of 406 (total:406,skipped:0) (95.81%) unit cell: 5.934(4) 5.935(4) 5.935(3) 60.05(7) 90.04(5) 60.00(7) V = 147.87(15) UB fit with 389 obs out of 406 (total:406,skipped:0) (95.81%) UB - matrix: -0.070230 0.031164 0.088378 ( 0.000079 0.000057 0.000059 ) -0.068440 -0.065604 -0.010634 ( 0.000081 0.000059 0.000060 ) 0.108717 -0.152526 0.116094 ( 0.000099 0.000072 0.000074 ) M - matrix: 0.021436 -0.014281 0.007142 ( 0.000027 0.000019 0.000017 ) -0.014281 0.028539 -0.014256 ( 0.000019 0.000024 0.000016 ) 0.007142 -0.014256 0.021402 ( 0.000017 0.000016 0.000020 ) unit cell: 5.934(4) 5.935(4) 5.935(3) 60.05(7) 90.04(5) 60.00(7) V = 147.87(15) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.070219 0.031164 0.088390 ( 0.000079 0.000057 0.000059 ) -0.068429 -0.065612 -0.010622 ( 0.000081 0.000059 0.000060 ) 0.108716 -0.152498 0.116085 ( 0.000099 0.000072 0.000074 ) M - matrix: 0.021432 -0.014278 0.007141 ( 0.000027 0.000019 0.000017 ) -0.014278 0.028532 -0.014251 ( 0.000019 0.000024 0.000016 ) 0.007141 -0.014251 0.021401 ( 0.000017 0.000016 0.000020 ) UB fit with 389 obs out of 406 (total:406,skipped:0) (95.81%) unit cell: 5.934(4) 5.935(4) 5.935(3) 60.06(7) 90.04(5) 60.00(7) V = 147.89(15) 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Run 2 Omega scan: (-103.000 - -28.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 585 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070219 0.031164 0.088390 ( 0.000079 0.000057 0.000059 ) -0.068429 -0.065612 -0.010622 ( 0.000081 0.000059 0.000060 ) 0.108716 -0.152498 0.116085 ( 0.000099 0.000072 0.000074 ) M - matrix: 0.021432 -0.014278 0.007141 ( 0.000027 0.000019 0.000017 ) -0.014278 0.028532 -0.014251 ( 0.000019 0.000024 0.000016 ) 0.007141 -0.014251 0.021401 ( 0.000017 0.000016 0.000020 ) UB fit with 389 obs out of 406 (total:406,skipped:0) (95.81%) unit cell: 5.934(4) 5.935(4) 5.935(3) 60.06(7) 90.04(5) 60.00(7) V = 147.89(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 388 obs out of 406 (total:406,skipped:0) (95.57%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb 5 of 312 peaks identified as outliers and rejected 307 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 307 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 307 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 1.28 | 31 | 0.971 ( 0.116) | 1.131 ( 0.439) | 1.096 ( 0.841) | 1.28- 1.09 | 31 | 1.015 ( 0.089) | 1.094 ( 0.129) | 1.007 ( 0.376) | 1.09- 0.96 | 31 | 1.020 ( 0.084) | 1.180 ( 0.450) | 1.096 ( 0.506) | 0.94- 0.84 | 31 | 1.006 ( 0.083) | 1.060 ( 0.135) | 1.079 ( 0.382) | 0.84- 0.78 | 31 | 1.000 ( 0.089) | 1.053 ( 0.151) | 1.025 ( 0.246) | 0.78- 0.73 | 31 | 0.992 ( 0.050) | 1.053 ( 0.153) | 1.139 ( 0.419) | 0.73- 0.69 | 31 | 0.958 ( 0.061) | 0.962 ( 0.177) | 1.047 ( 0.404) | 0.69- 0.66 | 31 | 0.958 ( 0.038) | 0.904 ( 0.094) | 1.239 ( 0.464) | 0.66- 0.63 | 31 | 0.921 ( 0.026) | 0.858 ( 0.045) | 1.194 ( 0.430) | 0.63- 0.59 | 28 | 0.886 ( 0.030) | 0.827 ( 0.065) | 1.228 ( 0.483) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.74- 0.59 | 307 | 0.973 ( 0.083) | 1.014 ( 0.255) | 1.114 ( 0.484) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 307 obs out of 307 (total:307,skipped:0) (100.00%) UB - matrix: -0.070210 0.031015 0.088709 ( 0.000036 0.000027 0.000031 ) -0.068219 -0.065865 -0.010319 ( 0.000039 0.000029 0.000033 ) 0.108946 -0.152481 0.116298 ( 0.000031 0.000024 0.000027 ) M - matrix: 0.021452 -0.014297 0.007146 ( 0.000010 0.000007 0.000006 ) -0.014297 0.028551 -0.014302 ( 0.000007 0.000008 0.000006 ) 0.007146 -0.014302 0.021501 ( 0.000006 0.000006 0.000008 ) unit cell: 5.9328(19) 5.939(2) 5.9239(16) 59.99(3) 89.94(2) 59.95(3) V = 147.53(7) OTKP changes: 307 1 1 1 OTKP changes: 307 1 1 1 OTKP changes: 307 1 1 1 UB - matrix: -0.070384 0.031176 0.088604 ( 0.000035 0.000026 0.000030 ) -0.068467 -0.065857 -0.010392 ( 0.000034 0.000026 0.000029 ) 0.109007 -0.152759 0.116316 ( 0.000027 0.000021 0.000023 ) M - matrix: 0.021524 -0.014337 0.007154 ( 0.000009 0.000006 0.000006 ) -0.014337 0.028644 -0.014321 ( 0.000006 0.000007 0.000005 ) 0.007154 -0.014321 0.021488 ( 0.000006 0.000005 0.000008 ) UB fit with 307 obs out of 307 (total:307,skipped:0) (100.00%) unit cell: 5.9215(18) 5.9281(17) 5.9257(15) 59.98(3) 89.95(2) 59.97(3) V = 147.06(6) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -28.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 581 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070384 0.031176 0.088604 ( 0.000035 0.000026 0.000030 ) -0.068467 -0.065857 -0.010392 ( 0.000034 0.000026 0.000029 ) 0.109007 -0.152759 0.116316 ( 0.000027 0.000021 0.000023 ) M - matrix: 0.021524 -0.014337 0.007154 ( 0.000009 0.000006 0.000006 ) -0.014337 0.028644 -0.014321 ( 0.000006 0.000007 0.000005 ) 0.007154 -0.014321 0.021488 ( 0.000006 0.000005 0.000008 ) UB fit with 307 obs out of 307 (total:307,skipped:0) (100.00%) unit cell: 5.9215(18) 5.9281(17) 5.9257(15) 59.98(3) 89.95(2) 59.97(3) V = 147.06(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 307 obs out of 307 (total:307,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb 4 of 313 peaks identified as outliers and rejected 309 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 309 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 309 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 31 | 0.974 ( 0.133) | 1.205 ( 0.610) | 1.137 ( 0.914) | 1.28- 1.09 | 31 | 1.015 ( 0.088) | 1.082 ( 0.117) | 0.989 ( 0.380) | 1.09- 0.96 | 31 | 1.016 ( 0.086) | 1.151 ( 0.419) | 1.105 ( 0.454) | 0.96- 0.85 | 31 | 0.995 ( 0.085) | 1.057 ( 0.130) | 1.032 ( 0.389) | 0.85- 0.81 | 31 | 1.007 ( 0.088) | 1.059 ( 0.152) | 1.009 ( 0.230) | 0.78- 0.73 | 31 | 0.989 ( 0.051) | 1.046 ( 0.144) | 1.193 ( 0.447) | 0.73- 0.70 | 31 | 0.962 ( 0.061) | 0.929 ( 0.122) | 1.199 ( 0.591) | 0.69- 0.66 | 31 | 0.957 ( 0.037) | 0.909 ( 0.092) | 1.277 ( 0.496) | 0.66- 0.63 | 31 | 0.926 ( 0.029) | 0.860 ( 0.046) | 1.176 ( 0.422) | 0.62- 0.59 | 30 | 0.886 ( 0.032) | 0.827 ( 0.064) | 1.207 ( 0.469) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 309 | 0.973 ( 0.085) | 1.013 ( 0.282) | 1.132 ( 0.516) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.5 | 75 | 1.113 ( 0.054) | 1.241 ( 0.417) | 1.199 ( 0.578) | 13.7-19.7 | 75 | 1.097 ( 0.067) | 1.162 ( 0.315) | 1.271 ( 0.546) | 19.7-23.6 | 75 | 1.089 ( 0.080) | 1.160 ( 0.300) | 1.226 ( 0.591) | 23.7-27.9 | 75 | 1.057 ( 0.095) | 1.135 ( 0.406) | 1.274 ( 0.549) | 27.9-31.3 | 75 | 1.029 ( 0.092) | 0.982 ( 0.108) | 1.205 ( 0.455) | 31.3-34.5 | 75 | 1.014 ( 0.098) | 0.930 ( 0.109) | 1.302 ( 0.542) | 34.5-37.2 | 75 | 0.985 ( 0.090) | 0.895 ( 0.090) | 1.276 ( 0.508) | 37.3-39.9 | 75 | 0.974 ( 0.113) | 0.899 ( 0.201) | 1.263 ( 0.617) | 40.0-42.8 | 75 | 0.939 ( 0.102) | 0.851 ( 0.100) | 1.108 ( 0.468) | 42.9-49.8 | 76 | 0.959 ( 0.096) | 0.827 ( 0.072) | 1.160 ( 0.473) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.8 | 751 | 1.026 ( 0.108) | 1.008 ( 0.286) | 1.228 ( 0.538) | Fitted profile normalization line parameters e1 dimension: a=-0.0043 b=1.15 e2 dimension: a=-0.0101 b=1.28 e3 dimension: a=0.0027 b=0.98 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5031 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 8359019 lp-corr: 2431524 PROFFITPEAK - Finished at Tue Mar 27 13:52:03 2018 PROFFITMAIN - Started at Tue Mar 27 13:52:03 2018 OTKP changes: 751 1 2 2 OTKP changes: 751 1 2 2 OTKP changes: 751 1 2 2 UB - matrix: -0.070388 0.031131 0.088756 ( 0.000023 0.000018 0.000014 ) -0.068455 -0.065885 -0.010690 ( 0.000025 0.000020 0.000016 ) 0.109269 -0.153141 0.116347 ( 0.000020 0.000016 0.000012 ) M - matrix: 0.021580 -0.014415 0.007198 ( 0.000006 0.000004 0.000004 ) -0.014415 0.028762 -0.014350 ( 0.000004 0.000006 0.000003 ) 0.007198 -0.014350 0.021529 ( 0.000004 0.000003 0.000004 ) UB fit with 751 obs out of 751 (total:751,skipped:0) (100.00%) unit cell: 5.9199(12) 5.9163(12) 5.9172(9) 60.079(19) 90.023(15) 59.92(2) V = 146.50(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070169 0.030738 0.088794 ( 0.000027 0.000026 0.000015 ) -0.068142 -0.066076 -0.010722 ( 0.000024 0.000024 0.000014 ) 0.109164 -0.153128 0.116153 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014370 0.007180 ( 0.000007 0.000005 0.000004 ) -0.014370 0.028759 -0.014348 ( 0.000005 0.000008 0.000004 ) 0.007180 -0.014348 0.021491 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9308(13) 5.9162(14) 5.9248(10) 60.05(2) 90.041(17) 59.96(2) V = 146.97(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070304 0.030870 0.088794 ( 0.000026 0.000026 0.000015 ) -0.068332 -0.066114 -0.010661 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153212 0.116262 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021559 -0.014399 0.007193 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028798 -0.014367 ( 0.000005 0.000008 0.000004 ) 0.007193 -0.014367 0.021515 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9114(13) 5.9216(10) 60.04(2) 90.040(16) 59.98(2) V = 146.51(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.843) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070304 0.030870 0.088794 ( 0.000026 0.000026 0.000015 ) -0.068332 -0.066114 -0.010661 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153212 0.116262 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021559 -0.014399 0.007193 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028798 -0.014367 ( 0.000005 0.000008 0.000004 ) 0.007193 -0.014367 0.021515 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9114(13) 5.9216(10) 60.04(2) 90.040(16) 59.98(2) V = 146.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070304 0.030870 0.088794 ( 0.000026 0.000026 0.000015 ) -0.068332 -0.066114 -0.010661 ( 0.000023 0.000023 0.000013 ) 0.109300 -0.153212 0.116262 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021559 -0.014399 0.007193 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028798 -0.014367 ( 0.000005 0.000008 0.000004 ) 0.007193 -0.014367 0.021515 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9114(13) 5.9216(10) 60.04(2) 90.040(16) 59.98(2) V = 146.51(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 309 obs out of 309 (total:309,skipped:0) (100.00%) UB - matrix: -0.070482 0.031245 0.088566 ( 0.000036 0.000027 0.000030 ) -0.068620 -0.065845 -0.010429 ( 0.000041 0.000030 0.000034 ) 0.109050 -0.152916 0.116331 ( 0.000030 0.000023 0.000026 ) M - matrix: 0.021568 -0.014359 0.007159 ( 0.000010 0.000007 0.000006 ) -0.014359 0.028695 -0.014335 ( 0.000007 0.000008 0.000006 ) 0.007159 -0.014335 0.021486 ( 0.000006 0.000006 0.000008 ) unit cell: 5.914(2) 5.922(2) 5.9264(16) 59.97(3) 89.94(2) 59.98(3) V = 146.77(7) OTKP changes: 309 1 1 1 OTKP changes: 309 1 1 1 OTKP changes: 309 1 1 1 UB - matrix: -0.070452 0.031267 0.088777 ( 0.000035 0.000027 0.000030 ) -0.068732 -0.065825 -0.010415 ( 0.000039 0.000030 0.000033 ) 0.109149 -0.153053 0.116525 ( 0.000029 0.000021 0.000024 ) M - matrix: 0.021601 -0.014384 0.007180 ( 0.000010 0.000006 0.000006 ) -0.014384 0.028736 -0.014373 ( 0.000006 0.000008 0.000006 ) 0.007180 -0.014373 0.021568 ( 0.000006 0.000006 0.000008 ) UB fit with 309 obs out of 309 (total:309,skipped:0) (100.00%) unit cell: 5.9106(19) 5.9189(19) 5.9152(16) 59.97(3) 89.94(2) 59.97(3) V = 146.29(7) Run 2 Omega scan: (-103.000 - -28.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.843) HKL list info: 571 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070452 0.031267 0.088777 ( 0.000035 0.000027 0.000030 ) -0.068732 -0.065825 -0.010415 ( 0.000039 0.000030 0.000033 ) 0.109149 -0.153053 0.116525 ( 0.000029 0.000021 0.000024 ) M - matrix: 0.021601 -0.014384 0.007180 ( 0.000010 0.000006 0.000006 ) -0.014384 0.028736 -0.014373 ( 0.000006 0.000008 0.000006 ) 0.007180 -0.014373 0.021568 ( 0.000006 0.000006 0.000008 ) UB fit with 309 obs out of 309 (total:309,skipped:0) (100.00%) unit cell: 5.9106(19) 5.9189(19) 5.9152(16) 59.97(3) 89.94(2) 59.97(3) V = 146.29(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 309 obs out of 309 (total:309,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070452 0.031267 0.088777 ( 0.000035 0.000027 0.000030 ) -0.068732 -0.065825 -0.010415 ( 0.000039 0.000030 0.000033 ) 0.109149 -0.153053 0.116525 ( 0.000029 0.000021 0.000024 ) M - matrix: 0.021601 -0.014384 0.007180 ( 0.000010 0.000006 0.000006 ) -0.014384 0.028736 -0.014373 ( 0.000006 0.000008 0.000006 ) 0.007180 -0.014373 0.021568 ( 0.000006 0.000006 0.000008 ) UB fit with 309 obs out of 309 (total:309,skipped:0) (100.00%) unit cell: 5.9106(19) 5.9189(19) 5.9152(16) 59.97(3) 89.94(2) 59.97(3) V = 146.29(7) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070360 0.031136 0.088770 ( 0.000024 0.000019 0.000015 ) -0.068462 -0.065889 -0.010654 ( 0.000025 0.000020 0.000015 ) 0.109253 -0.153044 0.116286 ( 0.000021 0.000017 0.000013 ) M - matrix: 0.021574 -0.014400 0.007188 ( 0.000007 0.000005 0.000004 ) -0.014400 0.028733 -0.014331 ( 0.000005 0.000006 0.000003 ) 0.007188 -0.014331 0.021516 ( 0.000004 0.000003 0.000004 ) UB fit with 751 obs out of 751 (total:751,skipped:0) (100.00%) unit cell: 5.9198(12) 5.9173(12) 5.9173(9) 60.096(19) 90.023(15) 59.92(2) V = 146.58(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 48 reflections under beam stop or inside a detector rejection region 8 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof 1047 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:52:06 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.843) Run 2 Omega scan: (-103.000 - -28.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.843) PROFFIT INFO: signal sum: min=271.0000 max=20212566.0000 PROFFIT INFO: signal sum lp corr: min=623.1977 max=2943729.1997 PROFFIT INFO: background sum: min=1049.0000 max=9025.0000 PROFFIT INFO: background sum sig2: min=597.0000 max=6302.0000 PROFFIT INFO: num of signal pixels: min=57 max=518 PROFFIT INFO: Inet: min=997.1162 max=4709967.0000 PROFFIT INFO: sig(Inet): min=180.3417 max=47415.5625 PROFFIT INFO: Inet/sig(Inet): min=1.09 max=229.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 5 30 89 216 238 391 678 944 1047 Percent 0.0 0.0 0.5 2.9 8.5 20.6 22.7 37.3 64.8 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4709967- 1326440 104 2067594.29 126.69 100.00 1325029- 785175 104 999782.87 111.38 100.00 781409- 315081 104 511155.31 96.50 100.00 315017- 186145 104 232543.08 75.05 100.00 185737- 146652 104 167751.11 54.84 100.00 145919- 109306 104 122889.45 37.52 100.00 108917- 82139 104 95264.84 31.20 100.00 81989- 6242 104 49610.87 21.34 100.00 6110- 3481 104 4637.88 5.81 100.00 3474- 997 111 2709.28 4.16 72.97 ------------------------------------------------------------------------------------ 4709967- 997 1047 422567.93 56.10 97.13 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 104 762185.20 88.67 100.00 1.28- 1.03 104 599438.97 65.14 98.08 1.03- 0.89 104 580724.23 68.65 99.04 0.89- 0.79 104 422742.52 57.91 97.12 0.78- 0.72 104 429315.82 62.32 99.04 0.72- 0.65 104 389685.85 56.56 99.04 0.65- 0.61 104 242153.31 39.75 94.23 0.61- 0.56 104 332419.58 48.25 94.23 0.56- 0.51 104 265063.48 41.03 93.27 0.51- 0.40 111 215863.13 34.20 97.30 ------------------------------------------------------------------------------------ 5.26- 0.40 1047 422567.93 56.10 97.13 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:52:06 2018 Sorting 1047 observations 206 unique observations with > 7.00 F2/sig(F2) 1047 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 74 184 Total number of frames 184 Maximum number of 206 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1047 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 74 184 Total number of frames 184 841 observations > 7.00 F2/sig(F2) 841 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 74 184 Total number of frames 184 Frame #58 of 184 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 4.0 (Out of 841 removed 83 = 758, unique = 191) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 758 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 74 184 Total number of frames 184 Frame #23 of 184 skipped from refinement Frame #58 of 184 skipped from refinement 2 frames need to be skipped from refinement, because of missing redundant and/or observable data 191 unique data precomputed (should be 191) 191 unique data with 758 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.0 (Out of 758 removed 0 = 758, unique = 191) 191 unique data precomputed (should be 191) 191 unique data with 758 observations RMS deviation of equivalent data = 0.68658 Rint = 0.66002 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.64027, wR= 4.10065 Trying model 1 (ne=2, no=0)... Results: Rint= 0.73806, wR= 2.99422, Acormin=-0.087, Acormax=1.908, Acor_av=0.612 F test: Probability=0.000, F= 0.746 Trying model 2 (ne=2, no=1)... Results: Rint= 0.86404, wR= 2.90901, Acormin=-0.381, Acormax=1.527, Acor_av=0.352 F test: Probability=0.000, F= 0.541 Trying model 3 (ne=4, no=0)... Results: Rint= 0.86203, wR= 2.54797, Acormin=-0.241, Acormax=2.138, Acor_av=0.355 F test: Probability=0.000, F= 0.538 Trying model 4 (ne=4, no=1)... Results: Rint= 0.90124, wR= 2.18985, Acormin=-1.165, Acormax=1.343, Acor_av=0.209 F test: Probability=0.000, F= 0.489 Trying model 5 (ne=4, no=3)... Results: Rint= 0.95621, wR= 2.60440, Acormin=-0.813, Acormax=0.880, Acor_av=0.039 F test: Probability=0.000, F= 0.429 Trying model 6 (ne=6, no=0)... Results: Rint= 0.91918, wR= 3.63281, Acormin=-1.267, Acormax=1.858, Acor_av=0.192 F test: Probability=0.000, F= 0.462 Trying model 7 (ne=6, no=1)... Results: Rint= 0.93584, wR= 2.39651, Acormin=-2.088, Acormax=0.998, Acor_av=0.080 F test: Probability=0.000, F= 0.443 Trying model 8 (ne=6, no=3)... Results: Rint= 0.97128, wR= 1.95340, Acormin=-0.933, Acormax=0.800, Acor_av=0.027 F test: Probability=0.000, F= 0.406 Trying model 9 (ne=6, no=5)... Results: Rint= 1.00205, wR= 1.95785, Acormin=-0.586, Acormax=0.697, Acor_av=0.008 F test: Probability=0.000, F= 0.373 Trying model 10 (ne=8, no=0)... Results: Rint= 1.05148, wR= 3.69891, Acormin=-0.692, Acormax=1.425, Acor_av=0.017 F test: Probability=0.000, F= 0.342 Trying model 11 (ne=8, no=1)... Results: Rint= 0.97846, wR= 3.15335, Acormin=-0.586, Acormax=0.509, Acor_av=0.001 F test: Probability=0.000, F= 0.392 Trying model 12 (ne=8, no=3)... Results: Rint= 0.93190, wR= 1.99298, Acormin=-0.039, Acormax=0.048, Acor_av=0.001 F test: Probability=0.000, F= 0.427 Trying model 13 (ne=8, no=5)... Results: Rint= 0.90760, wR= 1.80933, Acormin=-0.039, Acormax=0.039, Acor_av=0.001 F test: Probability=0.000, F= 0.440 Trying model 14 (ne=8, no=7)... Results: Rint= 0.93599, wR= 1.62501, Acormin=-0.025, Acormax=0.020, Acor_av=0.001 F test: Probability=0.000, F= 0.401 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.81014 There are 182 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 186 pars with 17391 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.68658 Using Levenberg-Marquardt: 0.00010 New wR= 0.66247 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.66002 with corrections 0.62997 Rint for all data: 0.81014 with corrections 0.79042 4 observations identified as outliers and rejected Cycle 2 wR= 0.65609 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64704 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.64027 with corrections 0.61111 Rint for all data: 0.81014 with corrections 0.79008 4 observations identified as outliers and rejected Cycle 3 wR= 0.62186 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61440 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.62328 with corrections 0.59762 Rint for all data: 0.81014 with corrections 0.79050 1 observations identified as outliers and rejected Cycle 4 wR= 0.61217 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60758 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.61261 with corrections 0.59479 Rint for all data: 0.81014 with corrections 0.79461 1 observations identified as outliers and rejected Cycle 5 wR= 0.60757 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60424 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.61176 with corrections 0.60219 Rint for all data: 0.81014 with corrections 0.79914 1 observations identified as outliers and rejected Final wR= 0.60424 Final frame scales: Min= 0.7801 Max= 5.9084 Final absorption correction factors: Amin= 0.3592 Amax= 1.5470 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 182 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 186 pars with 17391 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.75619 Using Levenberg-Marquardt: 0.00010 New wR= 0.64081 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.61015 with corrections 0.84257 Rint for all data: 0.81014 with corrections 0.96494 2 observations identified as outliers and rejected Cycle 2 wR= 0.63878 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61116 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60820 with corrections 0.96775 Rint for all data: 0.81014 with corrections 1.11456 1 observations identified as outliers and rejected Cycle 3 wR= 0.61093 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60308 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60511 with corrections 0.64839 Rint for all data: 0.81014 with corrections 0.82930 1 observations identified as outliers and rejected Cycle 4 wR= 0.60231 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59671 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60097 with corrections 0.63697 Rint for all data: 0.81014 with corrections 0.82561 0 observations identified as outliers and rejected Cycle 5 wR= 0.59671 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59372 There are 2 clusters with unrefined scales (size 1-1) Rint for refined data: 0.60097 with corrections 0.63785 Rint for all data: 0.81014 with corrections 0.82683 0 observations identified as outliers and rejected Final wR= 0.59372 Final frame scales: Min= 0.7001 Max= 7.9436 Final absorption correction factors: Amin= 0.1749 Amax= 1.8423 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 173 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 177 pars with 15753 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.78558 Using Levenberg-Marquardt: 0.00010 New wR= 0.66319 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.60097 with corrections 0.71776 Rint for all data: 0.81014 with corrections 0.89344 1 observations identified as outliers and rejected Cycle 2 wR= 0.64929 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61921 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.76660 Rint for all data: 0.81014 with corrections 0.94206 0 observations identified as outliers and rejected Cycle 3 wR= 0.62073 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60709 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.71523 Rint for all data: 0.81014 with corrections 0.89461 0 observations identified as outliers and rejected Cycle 4 wR= 0.60754 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60183 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.65098 Rint for all data: 0.81014 with corrections 0.84500 0 observations identified as outliers and rejected Cycle 5 wR= 0.60179 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59960 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.71696 Rint for all data: 0.81014 with corrections 0.87101 0 observations identified as outliers and rejected Final wR= 0.59960 Final frame scales: Min= 0.5155 Max= 3.4998 Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics There are 173 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 172 pars with 14878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74808 Using Levenberg-Marquardt: 0.00010 New wR= 0.63223 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.58647 Rint for all data: 0.81014 with corrections 0.80136 0 observations identified as outliers and rejected Cycle 2 wR= 0.62330 Using Levenberg-Marquardt: 0.00001 New wR= 0.60976 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59399 with corrections 0.95589 Rint for all data: 0.81014 with corrections 1.08084 2 observations identified as outliers and rejected Cycle 3 wR= 0.60517 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 New wR= 0.60399 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59241 with corrections 0.92175 Rint for all data: 0.81014 with corrections 1.05288 0 observations identified as outliers and rejected Cycle 4 wR= 0.60400 Using Levenberg-Marquardt: 10.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 100.00000 New wR= 0.60347 There are 7 clusters with unrefined scales (size 1-3) Rint for refined data: 0.59241 with corrections 0.90459 Rint for all data: 0.81014 with corrections 1.03849 Final wR= 0.60347 Frame scales out of range! Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 158 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 157 pars with 12403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 1.22476 Using Levenberg-Marquardt: 0.00010 New wR= 0.62062 There are 12 clusters with unrefined scales (size 1-5) Rint for refined data: 0.59241 with corrections 0.58752 Rint for all data: 0.81014 with corrections 0.80872 1 observations identified as outliers and rejected Cycle 2 wR= 0.60091 Using Levenberg-Marquardt: 0.00001 New wR= 0.59306 There are 12 clusters with unrefined scales (size 1-5) Rint for refined data: 0.59141 with corrections 0.58258 Rint for all data: 0.81014 with corrections 0.80428 1 observations identified as outliers and rejected Cycle 3 wR= 0.58261 Using Levenberg-Marquardt: 0.00000 New wR= 0.57842 There are 12 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58989 with corrections 0.58390 Rint for all data: 0.81014 with corrections 0.80630 0 observations identified as outliers and rejected Cycle 4 wR= 0.57786 Using Levenberg-Marquardt: 0.00000 New wR= 0.57650 There are 12 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58989 with corrections 0.58586 Rint for all data: 0.81014 with corrections 0.80628 0 observations identified as outliers and rejected Cycle 5 wR= 0.57626 Using Levenberg-Marquardt: 0.00000 New wR= 0.57761 Using Levenberg-Marquardt: 0.00000 New wR= 0.57761 Using Levenberg-Marquardt: 0.00000 New wR= 0.57761 Using Levenberg-Marquardt: 0.00001 New wR= 0.57760 Using Levenberg-Marquardt: 0.00010 New wR= 0.57753 Using Levenberg-Marquardt: 0.00100 New wR= 0.57691 Using Levenberg-Marquardt: 0.01000 New wR= 0.57491 There are 12 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58989 with corrections 0.58756 Rint for all data: 0.81014 with corrections 0.80665 0 observations identified as outliers and rejected Final wR= 0.57491 Final frame scales: Min= 1.0000 Max= 6.3538 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 147 active scales (one needs to be fixed) Refinement control: frame scale #70 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 146 pars with 10731 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.81834 Using Levenberg-Marquardt: 0.00010 New wR= 0.62602 There are 17 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58989 with corrections 0.60115 Rint for all data: 0.81014 with corrections 0.81137 1 observations identified as outliers and rejected Cycle 2 wR= 0.58530 Using Levenberg-Marquardt: 0.00001 New wR= 0.56967 There are 17 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58791 with corrections 0.58859 Rint for all data: 0.81014 with corrections 0.80421 0 observations identified as outliers and rejected Cycle 3 wR= 0.57330 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.57502 Using Levenberg-Marquardt: 1.00000 New wR= 0.57296 There are 17 clusters with unrefined scales (size 1-5) Rint for refined data: 0.58791 with corrections 0.58616 Rint for all data: 0.81014 with corrections 0.80292 Final wR= 0.57296 Final frame scales: Min= 0.6914 Max= 3.6484 3 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=965.1693 max=5315367.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.1242 max=56836.7617 PROFFIT INFO: 4 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/108 1043 reflections read from tmp file 849 reflections are rejected (710 as outliers, 139 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 58 22 3 Initial Chi^2= 0.98700 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.73373 Current error model SIG(F2)^2 = 489.76*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 359.36*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 359.36*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5315367- 1264516 104 2000562.11 80.05 100.00 1253999- 685970 104 934436.68 40.21 100.00 683285- 300602 104 488905.80 34.25 100.00 299040- 182839 104 237475.74 27.99 100.00 182387- 142186 104 160214.79 19.39 100.00 141998- 102688 104 121735.78 14.61 100.00 102254- 75666 104 88048.09 11.14 100.00 75650- 6521 104 45143.68 8.10 84.62 6472- 3294 104 4535.65 2.88 15.38 3290- 965 107 2422.25 2.40 11.21 ------------------------------------------------------------------------------------ 5315367- 965 1043 407180.49 24.04 80.92 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 104 773993.64 52.95 97.12 1.28- 1.03 104 580175.35 33.75 85.58 1.03- 0.89 104 559274.92 31.47 85.58 0.89- 0.78 104 386098.97 21.13 74.04 0.78- 0.72 104 383338.18 22.91 84.62 0.72- 0.65 104 360597.61 20.30 81.73 0.65- 0.61 104 225802.81 14.54 71.15 0.61- 0.56 104 305486.56 16.74 79.81 0.56- 0.51 104 256130.50 14.58 76.92 0.51- 0.40 107 245568.20 12.37 72.90 ------------------------------------------------------------------------------------ 5.26- 0.40 1043 407180.49 24.04 80.92 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 104 773993.64 52.95 97.12 5.26- 1.03 208 677084.50 43.35 91.35 5.26- 0.89 312 637814.64 39.39 89.42 5.26- 0.78 416 574885.72 34.82 85.58 5.26- 0.72 520 536576.21 32.44 85.38 5.26- 0.65 624 507246.45 30.42 84.78 5.26- 0.61 728 467040.21 28.15 82.83 5.26- 0.56 832 446846.01 26.72 82.45 5.26- 0.51 936 425655.39 25.37 81.84 5.26- 0.40 1043 407180.49 24.04 80.92 ------------------------------------------------------------------------------------ 5.26- 0.40 1043 407180.49 24.04 80.92 Scale applied to data: s=0.188134 (maximum obs:5315367.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.800; Rsigma 0.027: data 1043 -> merged 298 With outlier rejection... Rint 0.618; Rsigma 0.030: data 860 -> merged 298 Rejected total: 183, method kkm 180, method Blessing 3 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404388, 5.272569 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 3.53 100.00 53 1.46 - 1.12 15 15 6.20 100.00 93 1.08 - 0.96 15 15 5.07 100.00 76 0.96 - 0.86 15 15 4.53 100.00 68 0.86 - 0.79 15 15 4.27 100.00 64 0.79 - 0.73 15 15 4.20 100.00 63 0.73 - 0.69 15 15 3.27 100.00 49 0.69 - 0.65 15 15 3.20 100.00 48 0.65 - 0.63 15 15 2.33 100.00 35 0.63 - 0.60 21 21 2.90 100.00 61 --------------------------------------------------------------- 5.92 - 0.60 156 156 3.91 100.00 610 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:52:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919756 5.917315 5.917322 60.0957 90.0234 59.9223 860 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 412 467 413 437 646 580 584 860 N (int>3sigma) = 0 329 467 330 341 563 469 472 693 Mean intensity = 0.0 59.1 30.8 58.0 64.4 48.5 67.1 64.5 64.9 Mean int/sigma = 0.0 21.3 19.6 21.5 22.3 20.8 23.3 22.6 22.4 Lattice type: P chosen Volume: 146.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.912 5.917 5.917 60.10 60.04 60.06 Niggli form: a.a = 34.947 b.b = 35.015 c.c = 35.015 b.c = 17.457 a.c = 17.471 a.b = 17.459 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.177 [ 710] Vol = 586.3 Cell: 8.372 8.369 8.368 90.00 90.02 90.14 Volume: 586.31 Matrix: 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.118 RHOMBOHEDRAL R-lattice R(int) = 0.156 [ 470] Vol = 439.7 Cell: 5.920 5.918 14.483 90.04 89.96 119.92 Volume: 439.73 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.118 RHOMBOHEDRAL R-lattice R(int) = 0.120 [ 129] Vol = 439.7 Trigonal Cell: 5.920 5.918 14.483 90.04 89.96 119.92 Volume: 439.73 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.149 [ 473] Vol = 439.7 Cell: 5.912 5.920 14.507 90.07 90.00 119.98 Volume: 439.73 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.128 [ 138] Vol = 439.7 Trigonal Cell: 5.912 5.920 14.507 90.07 90.00 119.98 Volume: 439.73 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.015 ORTHORHOMBIC I-lattice R(int) = 0.149 [ 453] Vol = 293.2 Cell: 5.912 5.926 8.368 90.01 89.98 90.02 Volume: 293.15 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.196 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 507] Vol = 293.2 Cell: 5.917 8.369 5.920 89.91 90.02 90.10 Volume: 293.15 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.078 MONOCLINIC I-lattice R(int) = 0.139 [ 297] Vol = 293.2 Cell: 5.917 5.920 8.369 90.09 90.10 89.98 Volume: 293.15 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.012 MONOCLINIC I-lattice R(int) = 0.136 [ 313] Vol = 293.2 Cell: 5.912 5.926 8.368 89.99 90.02 90.02 Volume: 293.15 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.103 MONOCLINIC I-lattice R(int) = 0.120 [ 329] Vol = 293.2 Cell: 5.918 5.917 8.372 89.89 90.08 90.00 Volume: 293.15 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 83] Vol = 146.6 Cell: 5.912 5.917 5.917 60.10 60.04 60.06 Volume: 146.58 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 467 0 580 572 860 N (int>3sigma) = 0 0 0 0 467 0 469 458 693 Mean intensity = 0.0 0.0 0.0 0.0 30.8 0.0 67.1 67.1 64.9 Mean int/sigma = 0.0 0.0 0.0 0.0 19.6 0.0 23.3 22.6 22.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.097 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 11 11 60 206 N I>3s 10 10 21 206 0.8 0.8 0.8 35.1 5.4 5.4 3.4 23.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.177 669 Fd-3m 1 1 227 C N N N N 37 2284 0.182 705 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371787 8.368920 8.368369 90.0041 90.0236 90.1384 ZERR 1.00 0.002589 0.005848 0.000440 0.0191 0.0030 0.0039 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2925916- 872662 107 85 29 2.9 1195079.15 52.90 0.483 0.386 855043- 573600 127 115 29 4.0 608381.85 33.72 0.814 0.693 566218- 459628 139 107 29 3.7 432868.83 24.81 0.773 0.582 457771- 322583 115 88 29 3.0 284565.37 21.57 0.597 0.549 321333- 235962 130 105 29 3.6 188802.51 19.74 0.560 0.616 234170- 141998 118 94 29 3.2 142506.47 18.05 0.501 0.417 141946- 104156 80 68 29 2.3 129875.26 13.65 0.282 0.313 102499- 83053 89 76 29 2.6 88356.82 11.46 0.350 0.256 82370- 48130 72 61 29 2.1 66535.24 9.24 0.482 0.364 47401- 1512 66 61 37 1.6 16854.76 3.98 0.587 0.565 ------------------------------------------------------------------------------------------- 2925916- 1512 1043 860 298 2.9 345067.04 22.44 0.618 0.504 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 157 136 29 4.7 610712.21 45.09 0.692 0.576 0.015 1.12-0.87 180 145 29 5.0 415114.40 25.73 0.723 0.633 0.025 0.86-0.75 151 121 29 4.2 319613.04 21.00 0.545 0.409 0.034 0.74-0.67 127 98 29 3.4 329293.13 20.11 0.573 0.459 0.033 0.66-0.61 102 82 31 2.6 150171.99 12.10 0.571 0.483 0.053 0.61-0.57 95 82 30 2.7 354155.98 18.71 0.546 0.514 0.035 0.56-0.53 77 61 30 2.0 195157.03 13.02 0.372 0.327 0.048 0.53-0.50 68 57 29 2.0 129029.16 10.14 0.230 0.230 0.060 0.49-0.46 48 40 29 1.4 253247.14 14.27 0.394 0.401 0.048 0.46-0.40 38 38 33 1.2 311086.37 12.06 0.783 0.783 0.046 ------------------------------------------------------------------------------------------------------ inf-0.40 1043 860 298 2.9 345067.04 22.44 0.618 0.504 0.030 inf-0.60 747 610 156 3.9 393573.25 26.27 0.644 0.527 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 136 29 29 100.0 4.7 610712.21 118.30 0.692 0.008 1.12-0.87 145 29 29 100.0 5.0 415114.40 72.71 0.723 0.016 0.86-0.75 121 29 29 100.0 4.2 319613.04 50.59 0.545 0.020 0.74-0.67 98 29 29 100.0 3.4 329293.13 44.61 0.573 0.021 0.66-0.61 82 31 31 100.0 2.6 150171.99 24.25 0.571 0.037 0.61-0.57 82 35 30 85.7 2.7 354155.98 38.00 0.546 0.025 0.56-0.53 61 33 30 90.9 2.0 195157.03 21.46 0.372 0.034 0.53-0.50 57 46 29 63.0 2.0 129029.16 15.43 0.230 0.043 0.49-0.46 40 54 29 53.7 1.4 253247.14 18.41 0.394 0.037 0.46-0.40 38 146 33 22.6 1.2 311086.37 13.85 0.783 0.050 -------------------------------------------------------------------------------------------- inf-0.40 860 463 298 64.4 2.9 345067.04 53.12 0.618 0.021 inf-0.60 610 156 156 100.0 3.9 393573.25 66.53 0.644 0.016 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 -1.0 No constraint UB - matrix: -0.079565 -0.015568 -0.024773 ( 0.000011 0.000010 0.000011 ) -0.028904 0.032945 0.072502 ( 0.000011 0.000010 0.000011 ) -0.003517 0.076522 -0.036248 ( 0.000010 0.000008 0.000009 ) M - matrix: 0.007178 0.000017 0.000003 ( 0.000002 0.000001 0.000001 ) 0.000017 0.007183 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000001 0.007184 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.079565 -0.015568 -0.024773 ( 0.000011 0.000010 0.000011 ) -0.028904 0.032945 0.072502 ( 0.000011 0.000010 0.000011 ) -0.003517 0.076522 -0.036248 ( 0.000010 0.000008 0.000009 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3718(11) 8.3689(9) 8.3684(10) 90.004(9) 90.024(10) 90.138(9) V = 586.31(12) unit cell: 8.3697(3) 8.3697(3) 8.3697(3) 90.0 90.0 90.0 V = 586.31(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.843) Run 2 Omega scan: (-103.000 - -28.000,75 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.843) PROFFIT INFO: signal sum: min=271.0000 max=20212566.0000 PROFFIT INFO: signal sum lp corr: min=623.1977 max=2943729.1997 PROFFIT INFO: background sum: min=1049.0000 max=9025.0000 PROFFIT INFO: background sum sig2: min=597.0000 max=6302.0000 PROFFIT INFO: num of signal pixels: min=57 max=518 PROFFIT INFO: Inet: min=997.1162 max=4709967.0000 PROFFIT INFO: sig(Inet): min=180.3417 max=47415.5625 PROFFIT INFO: Inet/sig(Inet): min=1.09 max=229.79 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 10 60 178 432 476 782 1356 1888 2094 Percent 0.0 0.0 0.5 2.9 8.5 20.6 22.7 37.3 64.8 90.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4709967- 1326440 104 2067594.29 126.69 100.00 1325029- 785175 104 999782.87 111.38 100.00 781409- 315081 104 511155.31 96.50 100.00 315017- 186145 104 232543.08 75.05 100.00 185737- 146652 104 167751.11 54.84 100.00 145919- 109306 104 122889.45 37.52 100.00 108917- 82139 104 95264.84 31.20 100.00 81989- 6242 104 49610.87 21.34 100.00 6110- 3481 104 4637.88 5.81 100.00 3474- 997 111 2709.28 4.16 72.97 ------------------------------------------------------------------------------------ 4709967- 997 1047 422567.93 56.10 97.13 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 104 764612.99 84.87 100.00 1.32- 1.09 104 859957.05 76.72 100.00 1.09- 0.96 104 417132.30 67.69 100.00 0.96- 0.84 104 543190.00 74.55 98.08 0.84- 0.80 104 421678.29 63.64 100.00 0.80- 0.73 104 271431.61 44.21 100.00 0.73- 0.70 104 286500.14 42.98 87.50 0.70- 0.65 104 321975.24 48.27 98.08 0.65- 0.62 104 171804.78 29.47 90.38 0.62- 0.58 111 183488.74 30.33 97.30 ------------------------------------------------------------------------------------ 4.82- 0.58 1047 422567.93 56.10 97.13 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:52:07 2018 Sorting 1047 observations 82 unique observations with > 7.00 F2/sig(F2) 1047 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 74 184 Total number of frames 184 Maximum number of 82 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1047 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 24 62 Total number of frames 62 841 observations > 7.00 F2/sig(F2) 841 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 24 62 Total number of frames 62 Removing 'redundancy=1' reflections Average redundancy: 9.7 (Out of 841 removed 5 = 836, unique = 86) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 836 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 24 62 Total number of frames 62 86 unique data precomputed (should be 86) 86 unique data with 836 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 9.7 (Out of 836 removed 0 = 836, unique = 86) 86 unique data precomputed (should be 86) 86 unique data with 836 observations RMS deviation of equivalent data = 0.09006 Rint = 0.07355 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.07123, wR= 0.09327 Trying model 1 (ne=2, no=0)... Results: Rint= 0.04669, wR= 0.06066, Acormin=0.846, Acormax=1.198, Acor_av=0.988 F test: Probability=1.000, F= 2.312 Trying model 2 (ne=2, no=1)... Results: Rint= 0.04664, wR= 0.06066, Acormin=0.831, Acormax=1.183, Acor_av=0.985 F test: Probability=0.000, F= 0.998 Trying model 3 (ne=4, no=0)... Results: Rint= 0.03553, wR= 0.04752, Acormin=0.777, Acormax=1.184, Acor_av=0.950 F test: Probability=1.000, F= 1.705 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03078, wR= 0.04108, Acormin=0.687, Acormax=1.153, Acor_av=0.919 F test: Probability=1.000, F= 1.327 Trying model 5 (ne=4, no=3)... Results: Rint= 0.02863, wR= 0.03631, Acormin=0.671, Acormax=1.159, Acor_av=0.912 F test: Probability=0.966, F= 1.145 Trying model 6 (ne=6, no=0)... Results: Rint= 0.03342, wR= 0.04519, Acormin=0.755, Acormax=1.183, Acor_av=0.939 F test: Probability=0.000, F= 0.731 Trying model 7 (ne=6, no=1)... Results: Rint= 0.02911, wR= 0.03954, Acormin=0.690, Acormax=1.122, Acor_av=0.907 F test: Probability=0.000, F= 0.960 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02475, wR= 0.03225, Acormin=0.688, Acormax=1.279, Acor_av=0.925 F test: Probability=1.000, F= 1.314 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02198, wR= 0.02854, Acormin=0.775, Acormax=1.282, Acor_av=0.952 F test: Probability=0.998, F= 1.249 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03092, wR= 0.04213, Acormin=0.746, Acormax=1.176, Acor_av=0.934 F test: Probability=0.000, F= 0.508 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02598, wR= 0.03525, Acormin=0.695, Acormax=1.183, Acor_av=0.929 F test: Probability=0.000, F= 0.717 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02157, wR= 0.02817, Acormin=0.760, Acormax=1.290, Acor_av=0.953 F test: Probability=0.648, F= 1.029 Trying model 13 (ne=8, no=5)... Results: Rint= 0.01833, wR= 0.02418, Acormin=0.780, Acormax=1.270, Acor_av=0.963 F test: Probability=1.000, F= 1.403 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01709, wR= 0.02239, Acormin=0.775, Acormax=1.322, Acor_av=0.966 F test: Probability=0.937, F= 1.125 Final absorption model (ne=8, no=5): Rint= 0.01833, Acormin=0.780, Acormax=1.270, Acor_av=0.963 Combined refinement in use Rint: 0.07371 There are 62 active scales (one needs to be fixed) Refinement control: frame scale #24 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 5 (65 parameters) Refinement control: 126 pars with 8001 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.09006 Using Levenberg-Marquardt: 0.00010 New wR= 0.02004 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07355 with corrections 0.01600 Rint for all data: 0.07371 with corrections 0.01624 1 observations identified as outliers and rejected Cycle 2 wR= 0.02004 Using Levenberg-Marquardt: 0.00001 New wR= 0.01952 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07304 with corrections 0.01545 Rint for all data: 0.07371 with corrections 0.01570 0 observations identified as outliers and rejected Cycle 3 wR= 0.01952 Using Levenberg-Marquardt: 0.00000 New wR= 0.01949 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07304 with corrections 0.01548 Rint for all data: 0.07371 with corrections 0.01573 0 observations identified as outliers and rejected Cycle 4 wR= 0.01949 Using Levenberg-Marquardt: 0.00000 New wR= 0.01950 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07304 with corrections 0.01551 Rint for all data: 0.07371 with corrections 0.01576 Final wR= 0.01950 Final frame scales: Min= 0.9652 Max= 1.1761 Final absorption correction factors: Amin= 0.7249 Amax= 1.1948 PROFFIT INFO: Inet (after scale3 abspack): min=975.1929 max=4584326.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=178.1635 max=45471.7109 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/109 1047 reflections read from tmp file 23 reflections are rejected (22 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 7 9 0 10 5 8 8 53 Initial Chi^2= 0.26490 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.51956 Current error model SIG(F2)^2 = 122.99*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 186.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 186.89*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4584327- 1353807 104 2066327.06 114.25 100.00 1316206- 775757 104 990686.55 53.30 100.00 755994- 318966 104 512199.17 51.93 100.00 317817- 188482 104 229751.80 36.88 100.00 188407- 151323 104 168813.83 25.95 100.00 151267- 106708 104 120247.85 18.24 100.00 105797- 82666 104 95056.43 15.60 100.00 82570- 6119 104 50169.19 11.02 100.00 6033- 3434 104 4575.93 3.99 88.46 3410- 975 111 2707.70 3.30 56.76 ------------------------------------------------------------------------------------ 4584327- 975 1047 421236.53 33.24 94.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 104 767031.14 72.19 100.00 1.32- 1.09 104 861213.05 62.29 100.00 1.09- 0.96 104 422385.13 35.10 100.00 0.96- 0.84 104 536626.97 36.91 95.19 0.84- 0.80 104 421563.89 30.91 98.08 0.80- 0.73 104 269092.70 21.72 96.15 0.73- 0.70 104 285699.98 21.16 81.73 0.70- 0.65 104 315459.30 23.49 96.15 0.65- 0.62 104 170246.49 14.76 84.62 0.62- 0.58 111 179328.89 15.14 90.99 ------------------------------------------------------------------------------------ 4.82- 0.58 1047 421236.53 33.24 94.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.32 104 767031.14 72.19 100.00 4.82- 1.09 208 814122.10 67.24 100.00 4.82- 0.96 312 683543.11 56.53 100.00 4.82- 0.84 416 646814.07 51.62 98.80 4.82- 0.80 520 601764.04 47.48 98.65 4.82- 0.73 624 546318.81 43.19 98.24 4.82- 0.70 728 509087.55 40.04 95.88 4.82- 0.65 832 484884.02 37.97 95.91 4.82- 0.62 936 449924.29 35.39 94.66 4.82- 0.58 1047 421236.53 33.24 94.27 ------------------------------------------------------------------------------------ 4.82- 0.58 1047 421236.53 33.24 94.27 Scale applied to data: s=0.218134 (maximum obs:4584326.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.016; Rsigma 0.019: data 1047 -> merged 106 With outlier rejection... Rint 0.014; Rsigma 0.020: data 1038 -> merged 106 Rejected total: 9, method kkm 7, method Blessing 2 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585995, 4.832238 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 9 10 5.44 90.00 49 1.61 - 1.21 10 10 8.80 100.00 88 1.17 - 1.01 10 10 12.30 100.00 123 0.99 - 0.89 10 10 12.00 100.00 120 0.88 - 0.81 10 10 11.80 100.00 118 0.81 - 0.74 10 10 10.30 100.00 103 0.73 - 0.71 10 10 11.20 100.00 112 0.70 - 0.66 10 10 10.20 100.00 102 0.66 - 0.64 10 10 8.20 100.00 82 0.63 - 0.60 10 10 8.70 100.00 87 --------------------------------------------------------------- 5.92 - 0.60 99 100 9.94 99.00 984 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:52:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919756 5.917315 5.917322 60.0957 90.0234 59.9223 860 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 412 467 413 437 646 580 584 860 N (int>3sigma) = 0 329 467 330 341 563 469 472 693 Mean intensity = 0.0 59.1 30.8 58.0 64.4 48.5 67.1 64.5 64.9 Mean int/sigma = 0.0 21.3 19.6 21.5 22.3 20.8 23.3 22.6 22.4 Lattice type: P chosen Volume: 146.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.912 5.917 5.917 60.10 60.04 60.06 Niggli form: a.a = 34.947 b.b = 35.015 c.c = 35.015 b.c = 17.457 a.c = 17.471 a.b = 17.459 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.098 CUBIC F-lattice R(int) = 0.177 [ 710] Vol = 586.3 Cell: 8.372 8.369 8.368 90.00 90.02 90.14 Volume: 586.31 Matrix: 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.118 RHOMBOHEDRAL R-lattice R(int) = 0.156 [ 470] Vol = 439.7 Cell: 5.920 5.918 14.483 90.04 89.96 119.92 Volume: 439.73 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.118 RHOMBOHEDRAL R-lattice R(int) = 0.120 [ 129] Vol = 439.7 Trigonal Cell: 5.920 5.918 14.483 90.04 89.96 119.92 Volume: 439.73 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.149 [ 473] Vol = 439.7 Cell: 5.912 5.920 14.507 90.07 90.00 119.98 Volume: 439.73 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.128 [ 138] Vol = 439.7 Trigonal Cell: 5.912 5.920 14.507 90.07 90.00 119.98 Volume: 439.73 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000 -1.0000 2.0000 -3.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.015 ORTHORHOMBIC I-lattice R(int) = 0.149 [ 453] Vol = 293.2 Cell: 5.912 5.926 8.368 90.01 89.98 90.02 Volume: 293.15 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.196 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 507] Vol = 293.2 Cell: 5.917 8.369 5.920 89.91 90.02 90.10 Volume: 293.15 Matrix: 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.078 MONOCLINIC I-lattice R(int) = 0.139 [ 297] Vol = 293.2 Cell: 5.917 5.920 8.369 90.09 90.10 89.98 Volume: 293.15 Matrix: 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.012 MONOCLINIC I-lattice R(int) = 0.136 [ 313] Vol = 293.2 Cell: 5.912 5.926 8.368 89.99 90.02 90.02 Volume: 293.15 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.103 MONOCLINIC I-lattice R(int) = 0.120 [ 329] Vol = 293.2 Cell: 5.918 5.917 8.372 89.89 90.08 90.00 Volume: 293.15 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 83] Vol = 146.6 Cell: 5.912 5.917 5.917 60.10 60.04 60.06 Volume: 146.58 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 467 0 580 572 860 N (int>3sigma) = 0 0 0 0 467 0 469 458 693 Mean intensity = 0.0 0.0 0.0 0.0 30.8 0.0 67.1 67.1 64.9 Mean int/sigma = 0.0 0.0 0.0 0.0 19.6 0.0 23.3 22.6 22.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.097 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 11 11 60 206 N I>3s 10 10 21 206 0.8 0.8 0.8 35.1 5.4 5.4 3.4 23.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.177 669 Fd-3m 1 1 227 C N N N N 37 2284 0.182 705 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.371787 8.368920 8.368369 90.0041 90.0236 90.1384 ZERR 1.00 0.002589 0.005848 0.000440 0.0191 0.0030 0.0039 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4576709- 629016 236 232 26 8.9 1417264.83 76.98 0.012 0.013 611586- 144134 298 295 26 11.3 255827.05 37.12 0.017 0.018 129417- 66401 256 256 26 9.8 97006.03 15.38 0.029 0.035 43001- 2296 257 255 28 9.1 5893.69 4.48 0.095 0.121 ------------------------------------------------------------------------------------------- 4576709- 2296 1047 1038 106 9.8 414846.68 32.65 0.014 0.015 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 245 238 26 9.2 732385.44 61.20 0.014 0.013 0.011 1.01-0.78 295 295 26 11.3 445193.56 32.58 0.011 0.013 0.019 0.78-0.66 281 280 26 10.8 310999.62 22.92 0.016 0.017 0.028 0.66-0.59 226 225 28 8.0 168405.01 14.66 0.026 0.027 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 1047 1038 106 9.8 414846.68 32.65 0.014 0.015 0.020 inf-0.60 990 982 98 10.0 430559.58 33.73 0.014 0.015 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 238 27 26 96.3 9.2 732385.44 195.03 0.014 0.004 1.01-0.78 295 26 26 100.0 11.3 445193.56 115.26 0.011 0.006 0.78-0.66 280 26 26 100.0 10.8 310999.62 79.71 0.016 0.010 0.66-0.59 225 31 28 90.3 8.0 168405.01 44.95 0.026 0.016 -------------------------------------------------------------------------------------------- inf-0.59 1038 110 106 96.4 9.8 414846.68 108.72 0.014 0.007 inf-0.60 982 99 98 99.0 10.0 430559.58 112.66 0.014 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 13:59:18 2018) ID: 2932; threads 39; handles 878; mem 518392.00 (1237820.00)kB; time: 1w 4d 23h 4m 48s MEMORY INFO: Memory PF:243.0, Ph:423.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.2,peak PF: 697.1, WS: 297.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:244.0, Ph:423.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 697.1, WS: 299.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 13:59:18 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000024 0.000019 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000025 0.000020 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000021 0.000017 0.000013 ) 5.91502 ( 0.00122 ) 5.91640 ( 0.00123 ) 5.92265 ( 0.00092 ) 60.05206 ( 0.01910 ) 89.98756 ( 0.01471 ) 60.01743 ( 0.02171 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 13:59:18 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000024 0.000019 0.000015 ) -0.068858 -0.065594 -0.010716 ( 0.000025 0.000020 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000021 0.000017 0.000013 ) M - matrix: 0.021574 -0.014400 0.007188 ( 0.000007 0.000005 0.000004 ) -0.014400 0.028733 -0.014331 ( 0.000005 0.000006 0.000003 ) 0.007188 -0.014331 0.021516 ( 0.000004 0.000003 0.000004 ) unit cell: 5.9150(12) 5.9164(12) 5.9227(9) 60.052(19) 89.988(15) 60.02(2) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.083 ( 0.108) | 1.073 ( 0.135) | 1.145 ( 0.399) | 0.84- 0.81 | 44 | 1.105 ( 0.099) | 1.023 ( 0.124) | 1.367 ( 0.511) | 0.81- 0.73 | 44 | 1.095 ( 0.086) | 0.996 ( 0.125) | 1.322 ( 0.491) | 0.73- 0.69 | 44 | 1.089 ( 0.080) | 0.930 ( 0.110) | 1.402 ( 0.496) | 0.69- 0.66 | 44 | 1.080 ( 0.074) | 0.883 ( 0.089) | 1.388 ( 0.489) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.062 ( 0.110) | 0.998 ( 0.252) | 1.318 ( 0.893) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070035 0.030486 0.088658 ( 0.000027 0.000026 0.000015 ) -0.068374 -0.065763 -0.010700 ( 0.000027 0.000027 0.000015 ) 0.109065 -0.152749 0.115659 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028586 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9266(15) 5.9308(15) 5.9444(11) 60.01(2) 90.017(18) 60.02(3) V = 147.80(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070138 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9215(14) 5.9313(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070138 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9215(14) 5.9313(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.707) | 1.567 ( 2.300) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.170 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.142) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.029 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.993 ( 0.128) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.383 ( 0.483) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 45 | 1.005 ( 0.077) | 0.804 ( 0.035) | 1.278 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 441 | 1.063 ( 0.108) | 1.004 ( 0.281) | 1.323 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb PROFFITPEAK info: 1149 peaks in the peak location table UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) 535 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.4 | 85 | 1.119 ( 0.068) | 1.260 ( 0.452) | 1.345 ( 1.669) | 13.5-19.6 | 85 | 1.093 ( 0.066) | 1.160 ( 0.298) | 1.264 ( 0.552) | 19.6-23.4 | 85 | 1.082 ( 0.077) | 1.139 ( 0.274) | 1.187 ( 0.503) | 23.6-27.7 | 85 | 1.053 ( 0.094) | 1.144 ( 0.402) | 1.282 ( 0.648) | 27.7-31.2 | 85 | 1.032 ( 0.087) | 0.987 ( 0.105) | 1.221 ( 0.459) | 31.2-34.5 | 85 | 1.004 ( 0.099) | 0.934 ( 0.114) | 1.231 ( 0.523) | 34.5-37.0 | 85 | 0.974 ( 0.084) | 0.888 ( 0.086) | 1.287 ( 0.505) | 37.1-39.9 | 85 | 0.970 ( 0.110) | 0.900 ( 0.190) | 1.229 ( 0.599) | 39.9-42.9 | 86 | 0.939 ( 0.100) | 0.853 ( 0.101) | 1.135 ( 0.484) | 42.9-49.9 | 80 | 0.953 ( 0.091) | 0.828 ( 0.069) | 1.162 ( 0.460) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 846 | 1.022 ( 0.107) | 1.010 ( 0.287) | 1.235 ( 0.732) | Fitted profile normalization line parameters e1 dimension: a=-0.0044 b=1.15 e2 dimension: a=-0.0100 b=1.27 e3 dimension: a=0.0018 b=1.00 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706998 Maximum peak integral for reflections I/sig<= 10000 - raw: 9708196 lp-corr: 2429818 PROFFITPEAK - Finished at Tue Mar 27 13:59:31 2018 PROFFITMAIN - Started at Tue Mar 27 13:59:31 2018 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 OTKP changes: 846 1 2 2 DC PROFFIT INFO: potentially unstable global refinement UB - matrix: -0.070245 0.030980 0.088713 ( 0.000020 0.000016 0.000014 ) -0.068401 -0.065794 -0.010665 ( 0.000022 0.000018 0.000015 ) 0.109017 -0.152722 0.116031 ( 0.000020 0.000017 0.000014 ) M - matrix: 0.021498 -0.014325 0.007147 ( 0.000006 0.000004 0.000004 ) -0.014325 0.028612 -0.014271 ( 0.000004 0.000006 0.000003 ) 0.007147 -0.014271 0.021447 ( 0.000004 0.000003 0.000004 ) UB fit with 846 obs out of 846 (total:846,skipped:0) (100.00%) unit cell: 5.9261(11) 5.9259(11) 5.9253(8) 60.092(17) 90.010(13) 59.96(2) V = 147.24(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070118 0.030662 0.088780 ( 0.000026 0.000026 0.000015 ) -0.068218 -0.066001 -0.010691 ( 0.000023 0.000023 0.000013 ) 0.109126 -0.153024 0.116003 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021479 -0.014346 0.007163 ( 0.000007 0.000005 0.000004 ) -0.014346 0.028713 -0.014323 ( 0.000005 0.000008 0.000004 ) 0.007163 -0.014323 0.021453 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9293(13) 5.9196(13) 5.9299(10) 60.03(2) 90.026(16) 59.98(2) V = 147.18(4) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070133 0.030659 0.088733 ( 0.000026 0.000026 0.000015 ) -0.068213 -0.065963 -0.010737 ( 0.000023 0.000023 0.000013 ) 0.109138 -0.153012 0.116004 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9212(13) 5.9314(10) 60.04(2) 90.040(16) 59.98(2) V = 147.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070133 0.030659 0.088733 ( 0.000026 0.000026 0.000015 ) -0.068213 -0.065963 -0.010737 ( 0.000023 0.000023 0.000013 ) 0.109138 -0.153012 0.116004 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9212(13) 5.9314(10) 60.04(2) 90.040(16) 59.98(2) V = 147.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070133 0.030659 0.088733 ( 0.000026 0.000026 0.000015 ) -0.068213 -0.065963 -0.010737 ( 0.000023 0.000023 0.000013 ) 0.109138 -0.153012 0.116004 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028704 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021446 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(13) 5.9212(13) 5.9314(10) 60.04(2) 90.040(16) 59.98(2) V = 147.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070324 0.031149 0.088599 ( 0.000023 0.000020 0.000025 ) -0.068521 -0.065865 -0.010368 ( 0.000030 0.000026 0.000032 ) 0.108995 -0.152766 0.116313 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021521 -0.014328 0.007157 ( 0.000007 0.000005 0.000005 ) -0.014328 0.028646 -0.014326 ( 0.000005 0.000006 0.000005 ) 0.007157 -0.014326 0.021486 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9203(16) 5.9269(16) 5.9270(12) 59.97(2) 89.967(19) 60.01(3) V = 147.06(5) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070299 0.031118 0.088608 ( 0.000023 0.000020 0.000025 ) -0.068487 -0.065856 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.108980 -0.152734 0.116316 ( 0.000019 0.000017 0.000021 ) M - matrix: 0.021509 -0.014322 0.007157 ( 0.000007 0.000005 0.000005 ) -0.014322 0.028633 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007157 -0.014325 0.021488 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9221(16) 5.9287(16) 5.9271(12) 59.97(2) 89.966(19) 60.00(3) V = 147.13(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 725 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070299 0.031118 0.088608 ( 0.000023 0.000020 0.000025 ) -0.068487 -0.065856 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.108980 -0.152734 0.116316 ( 0.000019 0.000017 0.000021 ) M - matrix: 0.021509 -0.014322 0.007157 ( 0.000007 0.000005 0.000005 ) -0.014322 0.028633 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007157 -0.014325 0.021488 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9221(16) 5.9287(16) 5.9271(12) 59.97(2) 89.966(19) 60.00(3) V = 147.13(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070299 0.031118 0.088608 ( 0.000023 0.000020 0.000025 ) -0.068487 -0.065856 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.108980 -0.152734 0.116316 ( 0.000019 0.000017 0.000021 ) M - matrix: 0.021509 -0.014322 0.007157 ( 0.000007 0.000005 0.000005 ) -0.014322 0.028633 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007157 -0.014325 0.021488 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9221(16) 5.9287(16) 5.9271(12) 59.97(2) 89.966(19) 60.00(3) V = 147.13(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070243 0.030974 0.088680 ( 0.000020 0.000016 0.000014 ) -0.068383 -0.065762 -0.010700 ( 0.000022 0.000018 0.000016 ) 0.109015 -0.152694 0.116031 ( 0.000020 0.000017 0.000014 ) M - matrix: 0.021495 -0.014325 0.007152 ( 0.000006 0.000004 0.000004 ) -0.014325 0.028600 -0.014267 ( 0.000004 0.000006 0.000003 ) 0.007152 -0.014267 0.021442 ( 0.000004 0.000003 0.000004 ) UB fit with 846 obs out of 846 (total:846,skipped:0) (100.00%) unit cell: 5.9274(11) 5.9277(11) 5.9263(8) 60.098(17) 90.024(13) 59.96(2) V = 147.33(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 52 reflections under beam stop or inside a detector rejection region 9 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof 1182 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 13:59:34 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=321.0000 max=19914760.0000 PROFFIT INFO: signal sum lp corr: min=586.8505 max=2934201.7742 PROFFIT INFO: background sum: min=1062.0000 max=8272.0000 PROFFIT INFO: background sum sig2: min=590.0000 max=5889.0000 PROFFIT INFO: num of signal pixels: min=59 max=483 PROFFIT INFO: Inet: min=938.9608 max=4694723.0000 PROFFIT INFO: sig(Inet): min=96.3922 max=47431.1680 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.64 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 33 100 241 266 438 767 1068 1182 Percent 0.0 0.0 0.7 2.8 8.5 20.4 22.5 37.1 64.9 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1182 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1182 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4694723- 1318778 118 2044418.35 127.10 100.00 1309555- 785330 118 1002826.70 111.11 100.00 785174- 296411 118 503438.39 96.16 100.00 294813- 184382 118 225213.20 74.36 100.00 184118- 146668 118 166178.99 54.44 100.00 146568- 108750 118 123806.66 38.08 100.00 108629- 82216 118 95467.70 31.66 100.00 82046- 6099 118 49032.93 21.04 100.00 6072- 3447 118 4561.68 5.76 99.15 3441- 939 120 2590.55 4.25 73.33 ------------------------------------------------------------------------------------ 4694723- 939 1182 421044.27 56.31 97.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 118 777830.15 85.89 100.00 1.28- 1.03 118 565241.65 69.74 98.31 1.03- 0.90 118 540221.78 63.63 99.15 0.90- 0.81 118 389256.57 56.03 96.61 0.81- 0.74 118 494990.24 66.84 98.31 0.74- 0.67 118 406471.64 58.28 98.31 0.67- 0.61 118 225854.70 39.37 94.92 0.61- 0.56 118 357976.83 50.42 94.92 0.56- 0.51 118 251386.32 40.00 94.07 0.51- 0.40 120 204876.69 33.27 97.50 ------------------------------------------------------------------------------------ 5.27- 0.40 1182 421044.27 56.31 97.21 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:59:34 2018 Sorting 1182 observations 209 unique observations with > 7.00 F2/sig(F2) 1182 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 98 208 Total number of frames 208 Maximum number of 209 frame scales suggested for reliable scaling Glued frame scales: 1 frame = 1 scale 1182 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 98 208 Total number of frames 208 952 observations > 7.00 F2/sig(F2) 952 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 98 208 Total number of frames 208 Frame #58 of 208 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data Removing 'redundancy=1' reflections Average redundancy: 4.5 (Out of 952 removed 78 = 874, unique = 196) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 874 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 98 208 Total number of frames 208 Frame #58 of 208 skipped from refinement 1 frames need to be skipped from refinement, because of missing redundant and/or observable data 196 unique data precomputed (should be 196) 196 unique data with 874 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.5 (Out of 874 removed 0 = 874, unique = 196) 196 unique data precomputed (should be 196) 196 unique data with 874 observations RMS deviation of equivalent data = 0.68598 Rint = 0.66680 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.65291, wR= 3.95355 Trying model 1 (ne=2, no=0)... Results: Rint= 0.70709, wR= 3.22976, Acormin=-0.045, Acormax=2.073, Acor_av=0.656 F test: Probability=0.000, F= 0.846 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84066, wR= 3.23217, Acormin=-0.411, Acormax=1.748, Acor_av=0.423 F test: Probability=0.000, F= 0.596 Trying model 3 (ne=4, no=0)... Results: Rint= 0.81853, wR= 2.78231, Acormin=-0.258, Acormax=2.025, Acor_av=0.396 F test: Probability=0.000, F= 0.623 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86587, wR= 2.39399, Acormin=-0.878, Acormax=1.387, Acor_av=0.261 F test: Probability=0.000, F= 0.554 Trying model 5 (ne=4, no=3)... Results: Rint= 0.93519, wR= 2.24749, Acormin=-0.632, Acormax=0.982, Acor_av=0.044 F test: Probability=0.000, F= 0.470 Trying model 6 (ne=6, no=0)... Results: Rint= 0.90041, wR= 3.55834, Acormin=-1.086, Acormax=2.018, Acor_av=0.219 F test: Probability=0.000, F= 0.505 Trying model 7 (ne=6, no=1)... Results: Rint= 0.92387, wR= 3.03613, Acormin=-1.848, Acormax=1.317, Acor_av=0.106 F test: Probability=0.000, F= 0.477 Trying model 8 (ne=6, no=3)... Results: Rint= 0.98072, wR= 2.12187, Acormin=-0.894, Acormax=0.771, Acor_av=0.021 F test: Probability=0.000, F= 0.419 Trying model 9 (ne=6, no=5)... Results: Rint= 1.01156, wR= 2.67451, Acormin=-0.519, Acormax=1.201, Acor_av=0.009 F test: Probability=0.000, F= 0.387 Trying model 10 (ne=8, no=0)... Results: Rint= 1.03304, wR= 3.34814, Acormin=-0.716, Acormax=1.309, Acor_av=0.039 F test: Probability=0.000, F= 0.373 Trying model 11 (ne=8, no=1)... Results: Rint= 1.01132, wR= 2.86482, Acormin=-0.597, Acormax=0.652, Acor_av=0.001 F test: Probability=0.000, F= 0.388 Trying model 12 (ne=8, no=3)... Results: Rint= 0.94421, wR= 2.34269, Acormin=-0.037, Acormax=0.070, Acor_av=0.002 F test: Probability=0.000, F= 0.440 Trying model 13 (ne=8, no=5)... Results: Rint= 0.95117, wR= 2.00595, Acormin=-0.054, Acormax=0.057, Acor_av=0.001 F test: Probability=0.000, F= 0.426 Trying model 14 (ne=8, no=7)... Results: Rint= 0.98326, wR= 1.45375, Acormin=-0.062, Acormax=0.031, Acor_av=0.000 F test: Probability=0.000, F= 0.389 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.82367 There are 207 active scales (one needs to be fixed) Refinement control: frame scale #187 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 211 pars with 22366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.68598 Using Levenberg-Marquardt: 0.00010 New wR= 0.65967 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.66680 with corrections 0.63465 Rint for all data: 0.82367 with corrections 0.80062 3 observations identified as outliers and rejected Cycle 2 wR= 0.64491 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.63794 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.65291 with corrections 0.62065 Rint for all data: 0.82367 with corrections 0.79987 3 observations identified as outliers and rejected Cycle 3 wR= 0.62370 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61844 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.64240 with corrections 0.61392 Rint for all data: 0.82367 with corrections 0.80231 4 observations identified as outliers and rejected Cycle 4 wR= 0.61120 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60712 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.63732 with corrections 0.61499 Rint for all data: 0.82367 with corrections 0.80586 2 observations identified as outliers and rejected Cycle 5 wR= 0.60289 Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59989 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.63278 with corrections 0.61874 Rint for all data: 0.82367 with corrections 0.81053 2 observations identified as outliers and rejected Final wR= 0.59989 Final frame scales: Min= 0.4686 Max= 3.0377 Final absorption correction factors: Amin= 0.3476 Amax= 1.5939 3 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=568.4509 max=5339410.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=135.2754 max=68979.8672 PROFFIT INFO: 3 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/2 frame:1/108 1179 reflections read from tmp file 970 reflections are rejected (826 as outliers, 144 as groups of 1 refl) Redundancy: 1 2 3 4+ Number of groups: 0 61 21 6 Initial Chi^2= 0.62262 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94668 Current error model SIG(F2)^2 = 222.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 210.41*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 210.41*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5339411- 1262615 117 2030350.63 99.90 100.00 1255696- 674260 117 915884.53 59.39 100.00 664986- 291807 117 449768.19 43.80 100.00 291430- 190510 117 237306.29 34.74 100.00 190493- 141391 117 162985.74 24.16 100.00 139635- 105174 117 122073.88 20.65 100.00 104882- 68375 117 85827.01 15.82 100.00 68123- 7189 117 42621.65 11.45 97.44 7068- 3280 117 4582.36 3.82 76.92 3248- 568 126 2325.78 3.19 53.17 ------------------------------------------------------------------------------------ 5339411- 568 1179 402295.91 31.47 92.45 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 117 831495.98 68.90 99.15 1.28- 1.03 117 532572.03 43.95 97.44 1.03- 0.90 117 552539.58 39.46 97.44 0.90- 0.81 117 341149.62 28.19 88.89 0.81- 0.74 117 475938.35 30.88 94.02 0.74- 0.67 117 375846.95 28.15 95.73 0.67- 0.62 117 236028.77 19.09 87.18 0.62- 0.57 117 334071.55 23.40 88.89 0.57- 0.52 117 198421.41 18.24 88.89 0.52- 0.40 126 163280.66 15.69 87.30 ------------------------------------------------------------------------------------ 5.27- 0.40 1179 402295.91 31.47 92.45 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.27- 1.28 117 831495.98 68.90 99.15 5.27- 1.03 234 682034.01 56.43 98.29 5.27- 0.90 351 638869.20 50.77 98.01 5.27- 0.81 468 564439.30 45.12 95.73 5.27- 0.74 585 546739.11 42.27 95.38 5.27- 0.67 702 518257.09 39.92 95.44 5.27- 0.62 819 477938.76 36.94 94.26 5.27- 0.57 936 459955.35 35.25 93.59 5.27- 0.52 1053 430896.03 33.36 93.07 5.27- 0.40 1179 402295.91 31.47 92.45 ------------------------------------------------------------------------------------ 5.27- 0.40 1179 402295.91 31.47 92.45 Scale applied to data: s=0.187286 (maximum obs:5339410.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.809; Rsigma 0.021: data 1179 -> merged 298 With outlier rejection... Rint 0.652; Rsigma 0.022: data 983 -> merged 298 Rejected total: 196, method kkm 192, method Blessing 4 Completeness direct cell (a, b, c) = (5.282, 5.282, 5.282), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.405081, 5.281605 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.46 15 15 4.60 100.00 69 1.46 - 1.13 15 15 6.80 100.00 102 1.08 - 0.96 15 15 6.33 100.00 95 0.96 - 0.86 15 15 6.33 100.00 95 0.86 - 0.79 15 15 5.27 100.00 79 0.79 - 0.73 15 15 5.00 100.00 75 0.73 - 0.69 15 15 4.13 100.00 62 0.69 - 0.66 15 15 3.73 100.00 56 0.66 - 0.64 15 15 2.60 100.00 39 0.63 - 0.60 21 21 2.81 100.00 59 --------------------------------------------------------------- 5.93 - 0.60 156 156 4.69 100.00 731 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:59:35 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.927351 5.927722 5.926341 60.0976 90.0236 59.9584 983 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 471 535 464 508 735 651 668 983 N (int>3sigma) = 0 445 535 438 470 709 600 615 908 Mean intensity = 0.0 51.2 30.9 51.0 64.5 43.8 66.3 65.3 65.3 Mean int/sigma = 0.0 26.4 25.7 26.3 29.5 26.1 29.5 29.7 29.5 Lattice type: P chosen Volume: 147.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 Unitcell: 5.924 5.926 5.927 89.98 60.02 60.05 Niggli form: a.a = 35.092 b.b = 35.122 c.c = 35.133 b.c = 0.014 a.c = 17.544 a.b = 17.527 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.118 CUBIC F-lattice R(int) = 0.240 [ 832] Vol = 589.3 Cell: 8.380 8.388 8.384 89.88 89.99 90.02 Volume: 589.33 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 580] Vol = 442.0 Cell: 5.924 5.926 14.531 90.07 90.02 119.95 Volume: 442.00 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.193 [ 174] Vol = 442.0 Trigonal Cell: 5.924 5.926 14.531 90.07 90.02 119.95 Volume: 442.00 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.212 [ 613] Vol = 294.7 Cell: 5.928 5.929 8.384 89.93 89.91 89.94 Volume: 294.66 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.206 [ 577] Vol = 294.7 Cell: 5.929 5.928 8.384 89.91 89.93 89.94 Volume: 294.66 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.022 ORTHORHOMBIC I-lattice R(int) = 0.198 [ 559] Vol = 294.7 Cell: 5.924 8.380 5.936 90.00 89.97 90.02 Volume: 294.66 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.042 MONOCLINIC I-lattice R(int) = 0.180 [ 338] Vol = 294.7 Cell: 5.928 5.929 8.384 90.07 90.09 89.94 Volume: 294.66 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.018 MONOCLINIC I-lattice R(int) = 0.160 [ 310] Vol = 294.7 Cell: 5.924 8.380 5.936 90.00 90.03 90.02 Volume: 294.66 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.131 [ 119] Vol = 147.3 Cell: 5.924 5.926 5.927 89.98 60.02 60.05 Volume: 147.33 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 535 0 658 654 983 N (int>3sigma) = 0 0 0 0 535 0 610 605 908 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 68.3 68.6 65.3 Mean int/sigma = 0.0 0.0 0.0 0.0 25.7 0.0 29.8 30.1 29.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.114 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 69 221 N I>3s 9 9 57 221 0.8 0.8 0.8 35.1 6.9 6.9 4.2 31.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.240 782 Fd-3m 1 1 227 C N N N N 37 2284 0.246 819 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.380100 8.388438 8.383552 89.8844 89.9902 90.0165 ZERR 1.00 0.000410 0.005379 0.002356 0.0037 0.0028 0.0175 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3607108- 761261 150 125 29 4.3 1058642.42 64.37 0.549 0.506 760443- 551882 145 132 29 4.6 624675.06 41.01 0.829 0.678 546906- 409026 152 134 29 4.6 390806.71 35.76 0.826 0.782 406496- 295052 140 111 29 3.8 224687.13 25.32 0.605 0.582 286821- 218837 143 108 29 3.7 167589.89 24.58 0.563 0.526 214957- 137256 136 104 29 3.6 127712.56 18.26 0.476 0.512 137088- 91854 94 77 29 2.7 115556.11 18.12 0.227 0.155 91850- 66845 101 92 29 3.2 78338.37 13.02 0.636 0.488 66292- 43473 51 42 29 1.4 63283.62 13.08 0.244 0.256 42569- 1217 67 58 37 1.6 12439.31 4.84 0.485 0.490 ------------------------------------------------------------------------------------------- 3607108- 1217 1179 983 298 3.3 348893.12 29.54 0.652 0.572 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 192 160 29 5.5 622296.98 56.96 0.571 0.551 0.012 1.13-0.87 209 187 29 6.4 466786.29 34.75 0.885 0.870 0.019 0.86-0.75 176 152 29 5.2 354078.12 27.03 0.594 0.494 0.027 0.74-0.67 145 117 29 4.0 324417.97 26.18 0.620 0.560 0.025 0.66-0.61 116 91 32 2.8 125327.82 15.26 0.628 0.565 0.044 0.61-0.57 101 78 29 2.7 285960.54 21.90 0.463 0.416 0.030 0.56-0.53 79 60 29 2.1 140224.97 15.86 0.467 0.420 0.044 0.53-0.50 74 60 29 2.1 137447.94 14.26 0.485 0.448 0.041 0.50-0.47 49 40 30 1.3 186166.78 18.78 0.382 0.382 0.036 0.46-0.41 38 38 33 1.2 171363.41 15.78 0.792 0.792 0.038 ------------------------------------------------------------------------------------------------------ inf-0.41 1179 983 298 3.3 348893.12 29.54 0.652 0.572 0.022 inf-0.60 869 731 156 4.7 409005.79 33.90 0.672 0.604 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 160 29 29 100.0 5.5 622296.98 149.99 0.571 0.006 1.13-0.87 187 29 29 100.0 6.4 466786.29 107.09 0.885 0.011 0.86-0.75 152 29 29 100.0 5.2 354078.12 67.90 0.594 0.014 0.74-0.67 117 29 29 100.0 4.0 324417.97 64.00 0.620 0.016 0.66-0.61 91 32 32 100.0 2.8 125327.82 31.40 0.628 0.031 0.61-0.57 78 34 29 85.3 2.7 285960.54 40.98 0.463 0.020 0.56-0.53 60 32 29 90.6 2.1 140224.97 26.55 0.467 0.032 0.53-0.50 60 46 29 63.0 2.1 137447.94 23.36 0.485 0.032 0.50-0.47 40 55 30 54.5 1.3 186166.78 23.80 0.382 0.027 0.46-0.41 38 148 33 22.3 1.2 171363.41 18.13 0.792 0.038 -------------------------------------------------------------------------------------------- inf-0.41 983 464 298 64.2 3.3 348893.12 73.78 0.652 0.015 inf-0.60 731 156 156 100.0 4.7 409005.79 90.20 0.672 0.012 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 -2.0 1.0 -1.0 0.0 1.0 No constraint UB - matrix: -0.024705 -0.015487 0.079461 ( 0.000010 0.000008 0.000009 ) 0.072423 0.032881 0.028841 ( 0.000011 0.000009 0.000011 ) -0.036176 0.076347 0.003508 ( 0.000010 0.000008 0.000010 ) M - matrix: 0.007164 0.000002 -0.000001 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007150 -0.000014 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000014 0.007158 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024705 -0.015487 0.079461 ( 0.000010 0.000008 0.000009 ) 0.072423 0.032881 0.028841 ( 0.000011 0.000009 0.000011 ) -0.036176 0.076347 0.003508 ( 0.000010 0.000008 0.000010 ) M - matrix: 0.007157 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007157 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007157 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3801(10) 8.3884(9) 8.3835(9) 89.884(9) 89.990(10) 90.017(9) V = 589.33(12) unit cell: 8.3840(3) 8.3840(3) 8.3840(3) 90.0 90.0 90.0 V = 589.33(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) PROFFIT INFO: signal sum: min=321.0000 max=19914760.0000 PROFFIT INFO: signal sum lp corr: min=586.8505 max=2934201.7742 PROFFIT INFO: background sum: min=1062.0000 max=8272.0000 PROFFIT INFO: background sum sig2: min=590.0000 max=5889.0000 PROFFIT INFO: num of signal pixels: min=59 max=483 PROFFIT INFO: Inet: min=938.9608 max=4694723.0000 PROFFIT INFO: sig(Inet): min=96.3922 max=47431.1680 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.64 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 16 66 200 482 532 876 1534 2136 2364 Percent 0.0 0.0 0.7 2.8 8.5 20.4 22.5 37.1 64.9 90.4 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1182 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1182 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4694723- 1318778 118 2044418.35 127.10 100.00 1309555- 785330 118 1002826.70 111.11 100.00 785174- 296411 118 503438.39 96.16 100.00 294813- 184382 118 225213.20 74.36 100.00 184118- 146668 118 166178.99 54.44 100.00 146568- 108750 118 123806.66 38.08 100.00 108629- 82216 118 95467.70 31.66 100.00 82046- 6099 118 49032.93 21.04 100.00 6072- 3447 118 4561.68 5.76 99.15 3441- 939 120 2590.55 4.25 73.33 ------------------------------------------------------------------------------------ 4694723- 939 1182 421044.27 56.31 97.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 118 724443.92 85.31 100.00 1.39- 1.09 118 892211.31 76.43 100.00 1.09- 0.96 118 395538.50 67.36 100.00 0.96- 0.85 118 537503.93 74.77 97.46 0.85- 0.81 118 416212.72 63.39 100.00 0.81- 0.73 118 291991.73 46.27 100.00 0.73- 0.70 118 269155.37 40.90 86.44 0.70- 0.65 118 312157.37 47.13 98.31 0.65- 0.63 118 191775.77 31.74 92.37 0.63- 0.59 120 183478.63 30.22 97.50 ------------------------------------------------------------------------------------ 4.83- 0.59 1182 421044.27 56.31 97.21 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 13:59:35 2018 Sorting 1182 observations 81 unique observations with > 7.00 F2/sig(F2) 1182 observations in 2 runs Run # start # end # total # 1 0 108 109 2 0 98 208 Total number of frames 208 Maximum number of 81 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1182 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 32 70 Total number of frames 70 952 observations > 7.00 F2/sig(F2) 952 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 32 70 Total number of frames 70 Removing 'redundancy=1' reflections Average redundancy: 10.9 (Out of 952 removed 4 = 948, unique = 87) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 948 observations in 2 runs Run # start # end # total # 1 0 36 37 2 0 32 70 Total number of frames 70 87 unique data precomputed (should be 87) 87 unique data with 948 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 10.9 (Out of 948 removed 0 = 948, unique = 87) 87 unique data precomputed (should be 87) 87 unique data with 948 observations RMS deviation of equivalent data = 0.09902 Rint = 0.07923 0 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.07923, wR= 0.10426 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05570, wR= 0.07499, Acormin=0.813, Acormax=1.194, Acor_av=0.976 F test: Probability=1.000, F= 2.011 Trying model 2 (ne=2, no=1)... Results: Rint= 0.05587, wR= 0.07231, Acormin=0.774, Acormax=1.150, Acor_av=0.957 F test: Probability=0.000, F= 0.990 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04130, wR= 0.05544, Acormin=0.750, Acormax=1.166, Acor_av=0.937 F test: Probability=1.000, F= 1.800 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03497, wR= 0.04606, Acormin=0.697, Acormax=1.130, Acor_av=0.899 F test: Probability=1.000, F= 1.390 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03096, wR= 0.04029, Acormin=0.652, Acormax=1.167, Acor_av=0.897 F test: Probability=1.000, F= 1.265 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04004, wR= 0.05258, Acormin=0.755, Acormax=1.174, Acor_av=0.935 F test: Probability=0.000, F= 0.596 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03286, wR= 0.04400, Acormin=0.695, Acormax=1.135, Acor_av=0.892 F test: Probability=0.000, F= 0.882 Trying model 8 (ne=6, no=3)... Results: Rint= 0.02902, wR= 0.03719, Acormin=0.671, Acormax=1.281, Acor_av=0.908 F test: Probability=0.950, F= 1.121 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02640, wR= 0.03365, Acormin=0.715, Acormax=1.267, Acor_av=0.923 F test: Probability=0.994, F= 1.192 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03466, wR= 0.04695, Acormin=0.767, Acormax=1.199, Acor_av=0.960 F test: Probability=0.000, F= 0.583 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02948, wR= 0.04054, Acormin=0.702, Acormax=1.135, Acor_av=0.889 F test: Probability=0.000, F= 0.803 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02410, wR= 0.03176, Acormin=0.744, Acormax=1.323, Acor_av=0.932 F test: Probability=0.994, F= 1.191 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02132, wR= 0.02813, Acormin=0.758, Acormax=1.263, Acor_av=0.943 F test: Probability=0.999, F= 1.260 Trying model 14 (ne=8, no=7)... Results: Rint= 0.01981, wR= 0.02619, Acormin=0.756, Acormax=1.271, Acor_av=0.948 F test: Probability=0.964, F= 1.137 Final absorption model (ne=8, no=7): Rint= 0.01981, Acormin=0.756, Acormax=1.271, Acor_av=0.948 Combined refinement in use Rint: 0.07938 There are 70 active scales (one needs to be fixed) Refinement control: frame scale #24 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 149 pars with 11175 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.09902 Using Levenberg-Marquardt: 0.00010 New wR= 0.02187 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07923 with corrections 0.01736 Rint for all data: 0.07938 with corrections 0.01759 2 observations identified as outliers and rejected Cycle 2 wR= 0.02190 Using Levenberg-Marquardt: 0.00001 New wR= 0.02082 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07879 with corrections 0.01600 Rint for all data: 0.07938 with corrections 0.01628 0 observations identified as outliers and rejected Cycle 3 wR= 0.02082 Using Levenberg-Marquardt: 0.00000 New wR= 0.02065 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07879 with corrections 0.01579 Rint for all data: 0.07938 with corrections 0.01609 0 observations identified as outliers and rejected Cycle 4 wR= 0.02065 Using Levenberg-Marquardt: 0.00000 New wR= 0.02063 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07879 with corrections 0.01575 Rint for all data: 0.07938 with corrections 0.01604 0 observations identified as outliers and rejected Cycle 5 wR= 0.02063 Using Levenberg-Marquardt: 0.00000 New wR= 0.02061 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.07879 with corrections 0.01574 Rint for all data: 0.07938 with corrections 0.01602 0 observations identified as outliers and rejected Final wR= 0.02061 Final frame scales: Min= 0.9597 Max= 1.1161 Final absorption correction factors: Amin= 0.6751 Amax= 1.2261 PROFFIT INFO: Inet (after scale3 abspack): min=869.8019 max=4598126.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=118.9513 max=46124.2109 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/2 frame:1/109 1182 reflections read from tmp file 37 reflections are rejected (36 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 7 8 3 1 8 9 6 59 Initial Chi^2= 0.27711 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.45249 Current error model SIG(F2)^2 = 124.17*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 180.36*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 180.36*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4598126- 1334012 118 2064559.90 116.94 100.00 1328904- 751348 118 985827.52 54.27 100.00 747015- 311079 118 500841.97 52.38 100.00 310825- 186673 118 225030.54 36.62 100.00 186474- 151373 118 168179.66 26.55 100.00 150248- 105805 118 120414.55 18.89 100.00 105610- 83405 118 94615.92 15.91 100.00 83269- 5983 118 49202.94 11.02 100.00 5944- 3331 118 4472.24 4.01 90.68 3326- 870 120 2601.34 3.42 60.83 ------------------------------------------------------------------------------------ 4598126- 870 1182 420865.74 33.95 95.09 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 118 733499.91 72.08 100.00 1.39- 1.09 118 905781.08 65.06 100.00 1.09- 0.96 118 400668.12 35.28 98.31 0.96- 0.85 118 537085.86 37.58 95.76 0.85- 0.81 118 414052.00 31.33 98.31 0.81- 0.73 118 289370.14 23.09 98.31 0.73- 0.70 118 264932.77 20.55 83.05 0.70- 0.65 118 304102.08 23.38 96.61 0.65- 0.63 118 185764.84 16.08 88.14 0.63- 0.59 120 177524.98 15.36 92.50 ------------------------------------------------------------------------------------ 4.83- 0.59 1182 420865.74 33.95 95.09 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.83- 1.39 118 733499.91 72.08 100.00 4.83- 1.09 236 819640.50 68.57 100.00 4.83- 0.96 354 679983.04 57.47 99.44 4.83- 0.85 472 644258.74 52.50 98.52 4.83- 0.81 590 598217.39 48.27 98.47 4.83- 0.73 708 546742.85 44.07 98.45 4.83- 0.70 826 506484.27 40.71 96.25 4.83- 0.65 944 481186.50 38.54 96.29 4.83- 0.63 1062 448361.87 36.05 95.39 4.83- 0.59 1182 420865.74 33.95 95.09 ------------------------------------------------------------------------------------ 4.83- 0.59 1182 420865.74 33.95 95.09 Scale applied to data: s=0.217480 (maximum obs:4598126.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.016; Rsigma 0.019: data 1182 -> merged 106 With outlier rejection... Rint 0.015; Rsigma 0.019: data 1172 -> merged 106 Rejected total: 10, method kkm 7, method Blessing 3 Completeness direct cell (a, b, c) = (8.384, 8.384, 8.384), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586999, 4.840519 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.93 - 1.71 9 10 6.11 90.00 55 1.61 - 1.21 10 10 10.40 100.00 104 1.17 - 1.02 10 10 13.70 100.00 137 0.99 - 0.89 10 10 13.60 100.00 136 0.88 - 0.81 10 10 13.30 100.00 133 0.81 - 0.74 10 10 11.50 100.00 115 0.73 - 0.71 10 10 12.90 100.00 129 0.70 - 0.66 10 10 11.00 100.00 110 0.66 - 0.64 10 10 9.70 100.00 97 0.63 - 0.60 12 12 10.33 100.00 124 --------------------------------------------------------------- 5.93 - 0.60 101 102 11.29 99.02 1140 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 13:59:35 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.927351 5.927722 5.926341 60.0976 90.0236 59.9584 983 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 471 535 464 508 735 651 668 983 N (int>3sigma) = 0 445 535 438 470 709 600 615 908 Mean intensity = 0.0 51.2 30.9 51.0 64.5 43.8 66.3 65.3 65.3 Mean int/sigma = 0.0 26.4 25.7 26.3 29.5 26.1 29.5 29.7 29.5 Lattice type: P chosen Volume: 147.33 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 Unitcell: 5.924 5.926 5.927 89.98 60.02 60.05 Niggli form: a.a = 35.092 b.b = 35.122 c.c = 35.133 b.c = 0.014 a.c = 17.544 a.b = 17.527 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.118 CUBIC F-lattice R(int) = 0.240 [ 832] Vol = 589.3 Cell: 8.380 8.388 8.384 89.88 89.99 90.02 Volume: 589.33 Matrix:-1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 580] Vol = 442.0 Cell: 5.924 5.926 14.531 90.07 90.02 119.95 Volume: 442.00 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.193 [ 174] Vol = 442.0 Trigonal Cell: 5.924 5.926 14.531 90.07 90.02 119.95 Volume: 442.00 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.212 [ 613] Vol = 294.7 Cell: 5.928 5.929 8.384 89.93 89.91 89.94 Volume: 294.66 Matrix: 0.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.062 ORTHORHOMBIC I-lattice R(int) = 0.206 [ 577] Vol = 294.7 Cell: 5.929 5.928 8.384 89.91 89.93 89.94 Volume: 294.66 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.022 ORTHORHOMBIC I-lattice R(int) = 0.198 [ 559] Vol = 294.7 Cell: 5.924 8.380 5.936 90.00 89.97 90.02 Volume: 294.66 Matrix:-1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.042 MONOCLINIC I-lattice R(int) = 0.180 [ 338] Vol = 294.7 Cell: 5.928 5.929 8.384 90.07 90.09 89.94 Volume: 294.66 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.018 MONOCLINIC I-lattice R(int) = 0.160 [ 310] Vol = 294.7 Cell: 5.924 8.380 5.936 90.00 90.03 90.02 Volume: 294.66 Matrix: 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.131 [ 119] Vol = 147.3 Cell: 5.924 5.926 5.927 89.98 60.02 60.05 Volume: 147.33 Matrix: 1.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 535 0 658 654 983 N (int>3sigma) = 0 0 0 0 535 0 610 605 908 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 68.3 68.6 65.3 Mean int/sigma = 0.0 0.0 0.0 0.0 25.7 0.0 29.8 30.1 29.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.114 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 9 9 69 221 N I>3s 9 9 57 221 0.8 0.8 0.8 35.1 6.9 6.9 4.2 31.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.240 782 Fd-3m 1 1 227 C N N N N 37 2284 0.246 819 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.380100 8.388438 8.383552 89.8844 89.9902 90.0165 ZERR 1.00 0.000410 0.005379 0.002356 0.0037 0.0028 0.0175 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4564217- 619328 267 261 26 10.0 1413586.21 78.33 0.012 0.014 609573- 142047 342 339 26 13.0 250540.08 36.89 0.019 0.022 128419- 66594 286 286 26 11.0 96549.26 15.68 0.030 0.036 42714- 2142 287 286 28 10.2 5791.73 4.55 0.097 0.124 ------------------------------------------------------------------------------------------- 4564217- 2142 1182 1172 106 11.1 412242.84 33.05 0.015 0.017 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 280 271 26 10.4 720353.53 60.92 0.013 0.014 0.011 1.02-0.78 334 334 26 12.8 438720.23 33.02 0.011 0.014 0.019 0.78-0.66 313 312 26 12.0 311311.28 23.39 0.017 0.021 0.027 0.66-0.59 255 255 28 9.1 173612.26 15.31 0.029 0.031 0.040 ------------------------------------------------------------------------------------------------------ inf-0.59 1182 1172 106 11.1 412242.84 33.05 0.015 0.017 0.019 inf-0.60 1148 1138 100 11.4 419101.86 33.61 0.014 0.016 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 271 27 26 96.3 10.4 720353.53 208.48 0.013 0.004 1.02-0.78 334 26 26 100.0 12.8 438720.23 125.21 0.011 0.005 0.78-0.66 312 26 26 100.0 12.0 311311.28 86.53 0.017 0.009 0.66-0.59 255 31 28 90.3 9.1 173612.26 50.61 0.029 0.015 -------------------------------------------------------------------------------------------- inf-0.59 1172 110 106 96.4 11.1 412242.84 117.94 0.015 0.006 inf-0.60 1138 101 100 99.0 11.4 419101.86 120.40 0.014 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:06:13 2018) ID: 2932; threads 39; handles 878; mem 518392.00 (1237820.00)kB; time: 1w 4d 23h 11m 44s MEMORY INFO: Memory PF:246.0, Ph:425.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.2,peak PF: 697.1, WS: 297.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:248.0, Ph:425.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 697.1, WS: 299.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:06:13 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000020 0.000016 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000022 0.000018 0.000016 ) 0.109112 -0.153091 0.115835 ( 0.000020 0.000017 0.000014 ) 5.91502 ( 0.00112 ) 5.91640 ( 0.00114 ) 5.92265 ( 0.00083 ) 60.05206 ( 0.01733 ) 89.98756 ( 0.01329 ) 60.01743 ( 0.01993 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:06:13 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000020 0.000016 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000022 0.000018 0.000016 ) 0.109112 -0.153091 0.115835 ( 0.000020 0.000017 0.000014 ) M - matrix: 0.021495 -0.014325 0.007152 ( 0.000006 0.000004 0.000004 ) -0.014325 0.028600 -0.014267 ( 0.000004 0.000006 0.000003 ) 0.007152 -0.014267 0.021442 ( 0.000004 0.000003 0.000004 ) unit cell: 5.9150(11) 5.9164(11) 5.9227(8) 60.052(17) 89.988(13) 60.02(2) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb PROFFITPEAK info: 278 peaks in the peak location table UB fit with 132 obs out of 133 (total:133,skipped:0) (99.25%) UB - matrix: -0.070171 0.031187 0.089167 ( 0.000215 0.000103 0.000303 ) -0.068794 -0.065573 -0.010516 ( 0.000114 0.000055 0.000161 ) 0.108996 -0.152888 0.116037 ( 0.000092 0.000044 0.000130 ) M - matrix: 0.021537 -0.014342 0.007114 ( 0.000040 0.000020 0.000036 ) -0.014342 0.028647 -0.014270 ( 0.000020 0.000017 0.000027 ) 0.007114 -0.014270 0.021526 ( 0.000036 0.000027 0.000062 ) unit cell: 5.920(8) 5.920(7) 5.907(12) 60.12(16) 89.88(13) 59.89(13) V = 146.5(4) UB fit with 132 obs out of 133 (total:133,skipped:0) (99.25%) UB - matrix: -0.070171 0.031187 0.089167 ( 0.000215 0.000103 0.000303 ) -0.068794 -0.065573 -0.010516 ( 0.000114 0.000055 0.000161 ) 0.108996 -0.152888 0.116037 ( 0.000092 0.000044 0.000130 ) M - matrix: 0.021537 -0.014342 0.007114 ( 0.000040 0.000020 0.000036 ) -0.014342 0.028647 -0.014270 ( 0.000020 0.000017 0.000027 ) 0.007114 -0.014270 0.021526 ( 0.000036 0.000027 0.000062 ) unit cell: 5.920(8) 5.920(7) 5.907(12) 60.12(16) 89.88(13) 59.89(13) V = 146.5(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070181 0.031190 0.089191 ( 0.000218 0.000105 0.000307 ) -0.068776 -0.065587 -0.010522 ( 0.000115 0.000055 0.000162 ) 0.109013 -0.152916 0.116022 ( 0.000097 0.000047 0.000137 ) M - matrix: 0.021539 -0.014348 0.007112 ( 0.000040 0.000020 0.000036 ) -0.014348 0.028658 -0.014270 ( 0.000020 0.000017 0.000028 ) 0.007112 -0.014270 0.021527 ( 0.000036 0.000028 0.000063 ) UB fit with 131 obs out of 133 (total:133,skipped:0) (98.50%) unit cell: 5.920(8) 5.919(7) 5.906(12) 60.13(16) 89.87(13) 59.87(13) V = 146.5(4) UB fit with 131 obs out of 133 (total:133,skipped:0) (98.50%) UB - matrix: -0.070181 0.031190 0.089191 ( 0.000218 0.000105 0.000307 ) -0.068776 -0.065587 -0.010522 ( 0.000115 0.000055 0.000162 ) 0.109013 -0.152916 0.116022 ( 0.000097 0.000047 0.000137 ) M - matrix: 0.021539 -0.014348 0.007112 ( 0.000040 0.000020 0.000036 ) -0.014348 0.028658 -0.014270 ( 0.000020 0.000017 0.000028 ) 0.007112 -0.014270 0.021527 ( 0.000036 0.000028 0.000063 ) unit cell: 5.920(8) 5.919(7) 5.906(12) 60.13(16) 89.87(13) 59.87(13) V = 146.5(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070401 0.031221 0.089071 ( 0.000217 0.000105 0.000307 ) -0.068448 -0.066023 -0.010593 ( 0.000106 0.000051 0.000149 ) 0.108864 -0.152682 0.116039 ( 0.000094 0.000045 0.000133 ) M - matrix: 0.021493 -0.014300 0.007087 ( 0.000040 0.000020 0.000036 ) -0.014300 0.028646 -0.014237 ( 0.000020 0.000017 0.000027 ) 0.007087 -0.014237 0.021511 ( 0.000036 0.000027 0.000063 ) UB fit with 131 obs out of 133 (total:133,skipped:0) (98.50%) unit cell: 5.920(7) 5.910(6) 5.904(12) 60.19(16) 89.92(13) 59.95(12) V = 146.5(4) 133 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Run 3 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070401 0.031221 0.089071 ( 0.000217 0.000105 0.000307 ) -0.068448 -0.066023 -0.010593 ( 0.000106 0.000051 0.000149 ) 0.108864 -0.152682 0.116039 ( 0.000094 0.000045 0.000133 ) M - matrix: 0.021493 -0.014300 0.007087 ( 0.000040 0.000020 0.000036 ) -0.014300 0.028646 -0.014237 ( 0.000020 0.000017 0.000027 ) 0.007087 -0.014237 0.021511 ( 0.000036 0.000027 0.000063 ) UB fit with 131 obs out of 133 (total:133,skipped:0) (98.50%) unit cell: 5.920(7) 5.910(6) 5.904(12) 60.19(16) 89.92(13) 59.95(12) V = 146.5(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 131 obs out of 133 (total:133,skipped:0) (98.50%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb 2 of 93 peaks identified as outliers and rejected 91 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 91 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 91 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.60 | 9 | 0.957 ( 0.118) | 0.968 ( 0.131) | 1.028 ( 0.362) | 1.47- 1.17 | 9 | 1.052 ( 0.061) | 1.068 ( 0.066) | 0.844 ( 0.212) | 1.17- 1.04 | 9 | 1.069 ( 0.062) | 1.077 ( 0.047) | 0.910 ( 0.454) | 1.02- 0.92 | 9 | 1.035 ( 0.083) | 1.018 ( 0.083) | 1.074 ( 0.445) | 0.92- 0.82 | 9 | 1.075 ( 0.076) | 1.013 ( 0.079) | 1.194 ( 0.458) | 0.82- 0.75 | 9 | 1.046 ( 0.063) | 0.953 ( 0.074) | 1.495 ( 0.607) | 0.75- 0.71 | 9 | 1.012 ( 0.046) | 0.908 ( 0.102) | 1.345 ( 0.539) | 0.70- 0.67 | 9 | 0.993 ( 0.050) | 0.856 ( 0.057) | 1.337 ( 0.385) | 0.66- 0.62 | 9 | 0.978 ( 0.037) | 0.847 ( 0.027) | 1.242 ( 0.422) | 0.62- 0.59 | 10 | 0.949 ( 0.037) | 0.816 ( 0.038) | 1.113 ( 0.398) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 91 | 1.016 ( 0.080) | 0.951 ( 0.117) | 1.158 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) UB - matrix: -0.070262 0.031048 0.089060 ( 0.000114 0.000048 0.000164 ) -0.068018 -0.066414 -0.010615 ( 0.000084 0.000036 0.000121 ) 0.109039 -0.152859 0.116118 ( 0.000036 0.000015 0.000052 ) M - matrix: 0.021453 -0.014332 0.007126 ( 0.000021 0.000010 0.000019 ) -0.014332 0.028741 -0.014280 ( 0.000010 0.000007 0.000013 ) 0.007126 -0.014280 0.021528 ( 0.000019 0.000013 0.000032 ) unit cell: 5.930(5) 5.903(4) 5.904(6) 60.22(9) 90.02(8) 59.95(8) V = 146.5(2) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: -0.069932 0.031042 0.089014 ( 0.000111 0.000047 0.000160 ) -0.068700 -0.065720 -0.010235 ( 0.000026 0.000011 0.000037 ) 0.109010 -0.152847 0.116160 ( 0.000036 0.000015 0.000052 ) M - matrix: 0.021494 -0.014318 0.007141 ( 0.000018 0.000008 0.000017 ) -0.014318 0.028645 -0.014319 ( 0.000008 0.000006 0.000011 ) 0.007141 -0.014319 0.021521 ( 0.000017 0.000011 0.000031 ) UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) unit cell: 5.924(3) 5.925(2) 5.918(6) 60.01(7) 89.94(6) 59.98(5) V = 146.93(19) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb 1 of 92 peaks identified as outliers and rejected 91 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 91 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 91 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.61 | 9 | 1.078 ( 0.453) | 1.145 ( 0.613) | 1.066 ( 0.349) | 1.61- 1.26 | 9 | 1.070 ( 0.049) | 1.089 ( 0.041) | 0.933 ( 0.181) | 1.17- 1.09 | 9 | 1.049 ( 0.072) | 1.059 ( 0.070) | 0.725 ( 0.142) | 1.05- 0.92 | 9 | 1.037 ( 0.086) | 1.028 ( 0.085) | 1.069 ( 0.435) | 0.92- 0.82 | 9 | 1.078 ( 0.076) | 1.023 ( 0.083) | 1.147 ( 0.390) | 0.82- 0.75 | 9 | 1.047 ( 0.064) | 0.954 ( 0.076) | 1.481 ( 0.610) | 0.75- 0.71 | 9 | 1.013 ( 0.046) | 0.908 ( 0.101) | 1.345 ( 0.538) | 0.70- 0.67 | 9 | 0.994 ( 0.051) | 0.856 ( 0.058) | 1.331 ( 0.384) | 0.66- 0.62 | 9 | 0.982 ( 0.033) | 0.855 ( 0.015) | 1.254 ( 0.409) | 0.62- 0.59 | 10 | 0.947 ( 0.037) | 0.812 ( 0.039) | 1.100 ( 0.391) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 91 | 1.029 ( 0.159) | 0.971 ( 0.230) | 1.145 ( 0.455) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.6 | 94 | 1.128 ( 0.136) | 1.267 ( 0.483) | 1.176 ( 0.570) | 13.1-19.4 | 94 | 1.092 ( 0.064) | 1.155 ( 0.284) | 1.217 ( 0.532) | 19.5-23.4 | 94 | 1.082 ( 0.074) | 1.130 ( 0.263) | 1.174 ( 0.494) | 23.4-27.4 | 94 | 1.048 ( 0.092) | 1.115 ( 0.366) | 1.285 ( 0.615) | 27.5-31.1 | 94 | 1.036 ( 0.088) | 1.001 ( 0.168) | 1.254 ( 0.517) | 31.1-34.3 | 94 | 1.002 ( 0.096) | 0.934 ( 0.110) | 1.229 ( 0.516) | 34.3-37.0 | 94 | 0.973 ( 0.084) | 0.890 ( 0.090) | 1.263 ( 0.499) | 37.1-39.9 | 94 | 0.970 ( 0.106) | 0.896 ( 0.182) | 1.207 ( 0.579) | 39.9-42.8 | 94 | 0.939 ( 0.098) | 0.849 ( 0.099) | 1.168 ( 0.487) | 42.9-49.9 | 92 | 0.956 ( 0.088) | 0.827 ( 0.066) | 1.158 ( 0.460) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 938 | 1.023 ( 0.113) | 1.007 ( 0.286) | 1.213 ( 0.531) | Fitted profile normalization line parameters e1 dimension: a=-0.0044 b=1.15 e2 dimension: a=-0.0099 b=1.27 e3 dimension: a=0.0020 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 9708196 lp-corr: 2429818 PROFFITPEAK - Finished at Tue Mar 27 14:06:27 2018 PROFFITMAIN - Started at Tue Mar 27 14:06:27 2018 OTKP changes: 938 2 3 3 OTKP changes: 938 2 3 3 UB - matrix: -0.070308 0.031087 0.088805 ( 0.000019 0.000015 0.000013 ) -0.068601 -0.065818 -0.010676 ( 0.000022 0.000017 0.000015 ) 0.109201 -0.153104 0.116340 ( 0.000016 0.000013 0.000011 ) M - matrix: 0.021574 -0.014390 0.007193 ( 0.000005 0.000004 0.000003 ) -0.014390 0.028739 -0.014349 ( 0.000004 0.000005 0.000003 ) 0.007193 -0.014349 0.021535 ( 0.000003 0.000003 0.000004 ) UB fit with 938 obs out of 938 (total:938,skipped:0) (100.00%) unit cell: 5.9171(11) 5.9160(11) 5.9167(8) 60.064(16) 90.035(12) 59.968(19) V = 146.48(4) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070114 0.030704 0.088872 ( 0.000027 0.000027 0.000016 ) -0.068189 -0.066106 -0.010621 ( 0.000024 0.000024 0.000014 ) 0.109121 -0.153095 0.116070 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021473 -0.014351 0.007159 ( 0.000007 0.000005 0.000004 ) -0.014351 0.028751 -0.014339 ( 0.000005 0.000008 0.000004 ) 0.007159 -0.014339 0.021483 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9294(14) 5.9151(14) 5.9248(11) 60.03(2) 90.006(17) 59.98(2) V = 146.96(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070278 0.030872 0.088783 ( 0.000026 0.000026 0.000015 ) -0.068371 -0.066082 -0.010709 ( 0.000023 0.000023 0.000013 ) 0.109282 -0.153222 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021556 -0.014396 0.007201 ( 0.000007 0.000005 0.000004 ) -0.014396 0.028797 -0.014369 ( 0.000005 0.000008 0.000004 ) 0.007201 -0.014369 0.021519 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9106(13) 5.9212(10) 60.05(2) 90.070(16) 60.00(2) V = 146.50(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.842) HKL list info: 807 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070278 0.030872 0.088783 ( 0.000026 0.000026 0.000015 ) -0.068371 -0.066082 -0.010709 ( 0.000023 0.000023 0.000013 ) 0.109282 -0.153222 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021556 -0.014396 0.007201 ( 0.000007 0.000005 0.000004 ) -0.014396 0.028797 -0.014369 ( 0.000005 0.000008 0.000004 ) 0.007201 -0.014369 0.021519 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9106(13) 5.9212(10) 60.05(2) 90.070(16) 60.00(2) V = 146.50(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070278 0.030872 0.088783 ( 0.000026 0.000026 0.000015 ) -0.068371 -0.066082 -0.010709 ( 0.000023 0.000023 0.000013 ) 0.109282 -0.153222 0.116286 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021556 -0.014396 0.007201 ( 0.000007 0.000005 0.000004 ) -0.014396 0.028797 -0.014369 ( 0.000005 0.000008 0.000004 ) 0.007201 -0.014369 0.021519 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9192(13) 5.9106(13) 5.9212(10) 60.05(2) 90.070(16) 60.00(2) V = 146.50(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070397 0.031270 0.088593 ( 0.000024 0.000021 0.000026 ) -0.068604 -0.065922 -0.010331 ( 0.000031 0.000027 0.000033 ) 0.109022 -0.152790 0.116287 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021548 -0.014336 0.007150 ( 0.000007 0.000005 0.000005 ) -0.014336 0.028668 -0.014316 ( 0.000005 0.000007 0.000005 ) 0.007150 -0.014316 0.021478 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9152(16) 5.9217(16) 5.9255(13) 60.00(2) 89.96(2) 60.01(3) V = 146.83(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070340 0.031172 0.088794 ( 0.000023 0.000020 0.000025 ) -0.068712 -0.065862 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109123 -0.153060 0.116513 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021577 -0.014370 0.007179 ( 0.000007 0.000005 0.000005 ) -0.014370 0.028737 -0.014384 ( 0.000005 0.000006 0.000005 ) 0.007179 -0.014384 0.021567 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9126(16) 5.9194(16) 5.9177(12) 59.94(2) 89.947(19) 60.00(3) V = 146.40(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.842) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070340 0.031172 0.088794 ( 0.000023 0.000020 0.000025 ) -0.068712 -0.065862 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109123 -0.153060 0.116513 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021577 -0.014370 0.007179 ( 0.000007 0.000005 0.000005 ) -0.014370 0.028737 -0.014384 ( 0.000005 0.000006 0.000005 ) 0.007179 -0.014384 0.021567 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9126(16) 5.9194(16) 5.9177(12) 59.94(2) 89.947(19) 60.00(3) V = 146.40(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070340 0.031172 0.088794 ( 0.000023 0.000020 0.000025 ) -0.068712 -0.065862 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109123 -0.153060 0.116513 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021577 -0.014370 0.007179 ( 0.000007 0.000005 0.000005 ) -0.014370 0.028737 -0.014384 ( 0.000005 0.000006 0.000005 ) 0.007179 -0.014384 0.021567 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9126(16) 5.9194(16) 5.9177(12) 59.94(2) 89.947(19) 60.00(3) V = 146.40(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) UB - matrix: -0.070049 0.031045 0.089125 ( 0.000118 0.000050 0.000169 ) -0.068487 -0.065913 -0.010382 ( 0.000040 0.000017 0.000057 ) 0.109175 -0.152941 0.115966 ( 0.000078 0.000033 0.000111 ) M - matrix: 0.021516 -0.014358 0.007128 ( 0.000024 0.000014 0.000022 ) -0.014358 0.028699 -0.014285 ( 0.000014 0.000011 0.000019 ) 0.007128 -0.014285 0.021499 ( 0.000022 0.000019 0.000040 ) unit cell: 5.925(4) 5.916(3) 5.913(6) 60.12(8) 89.93(7) 59.89(6) V = 146.7(2) OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 OTKP changes: 91 1 1 1 UB - matrix: -0.070123 0.030967 0.089292 ( 0.000118 0.000050 0.000168 ) -0.068757 -0.065812 -0.010413 ( 0.000028 0.000012 0.000039 ) 0.109333 -0.153126 0.116170 ( 0.000075 0.000032 0.000106 ) M - matrix: 0.021598 -0.014388 0.007156 ( 0.000024 0.000013 0.000022 ) -0.014388 0.028738 -0.014338 ( 0.000013 0.000010 0.000018 ) 0.007156 -0.014338 0.021577 ( 0.000022 0.000018 0.000039 ) UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) unit cell: 5.912(3) 5.914(3) 5.906(6) 60.06(8) 89.91(7) 59.92(5) V = 146.1(2) Run 3 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.842) HKL list info: 266 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.070123 0.030967 0.089292 ( 0.000118 0.000050 0.000168 ) -0.068757 -0.065812 -0.010413 ( 0.000028 0.000012 0.000039 ) 0.109333 -0.153126 0.116170 ( 0.000075 0.000032 0.000106 ) M - matrix: 0.021598 -0.014388 0.007156 ( 0.000024 0.000013 0.000022 ) -0.014388 0.028738 -0.014338 ( 0.000013 0.000010 0.000018 ) 0.007156 -0.014338 0.021577 ( 0.000022 0.000018 0.000039 ) UB fit with 91 obs out of 91 (total:91,skipped:0) (100.00%) unit cell: 5.912(3) 5.914(3) 5.906(6) 60.06(8) 89.91(7) 59.92(5) V = 146.1(2) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070297 0.031083 0.088787 ( 0.000019 0.000015 0.000013 ) -0.068582 -0.065806 -0.010678 ( 0.000022 0.000017 0.000015 ) 0.109184 -0.153037 0.116311 ( 0.000017 0.000013 0.000012 ) M - matrix: 0.021566 -0.014381 0.007190 ( 0.000005 0.000004 0.000003 ) -0.014381 0.028717 -0.014337 ( 0.000004 0.000005 0.000003 ) 0.007190 -0.014337 0.021525 ( 0.000003 0.000003 0.000004 ) UB fit with 938 obs out of 938 (total:938,skipped:0) (100.00%) unit cell: 5.9181(11) 5.9178(11) 5.9176(8) 60.072(16) 90.040(13) 59.969(19) V = 146.59(4) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 56 reflections under beam stop or inside a detector rejection region 9 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof 1319 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:06:31 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.842) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.842) Run 3 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.842) PROFFIT INFO: signal sum: min=256.0000 max=20754984.0000 PROFFIT INFO: signal sum lp corr: min=585.5218 max=2944240.9465 PROFFIT INFO: background sum: min=1061.0000 max=15205.0000 PROFFIT INFO: background sum sig2: min=607.0000 max=7484.0000 PROFFIT INFO: num of signal pixels: min=55 max=496 PROFFIT INFO: Inet: min=936.8349 max=4710785.5000 PROFFIT INFO: sig(Inet): min=96.9086 max=47420.0703 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=229.29 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 44 122 272 298 500 863 1194 1319 Percent 0.0 0.0 0.6 3.3 9.2 20.6 22.6 37.9 65.4 90.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1319 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1319 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4710786- 1280771 131 2014368.86 126.43 100.00 1273872- 772396 131 986431.54 110.04 100.00 771621- 284659 131 490270.71 94.72 100.00 283576- 182599 131 219439.66 74.34 100.00 181919- 143303 131 163150.96 53.36 100.00 142478- 107378 131 121303.55 38.67 100.00 107377- 81765 131 93569.66 31.15 100.00 81732- 6335 131 50786.35 21.91 100.00 6321- 3428 131 4581.49 5.62 98.47 3424- 937 140 2543.00 4.17 70.00 ------------------------------------------------------------------------------------ 4710786- 937 1319 411832.66 55.69 96.66 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 131 762747.51 87.53 99.24 1.41- 1.07 131 609137.59 69.88 97.71 1.07- 0.93 131 463749.90 62.50 96.95 0.93- 0.82 131 402290.61 55.66 96.18 0.82- 0.74 131 432107.92 59.02 97.71 0.74- 0.67 131 395622.47 55.39 96.95 0.67- 0.62 131 296052.16 48.57 97.71 0.62- 0.57 131 314655.30 46.57 92.37 0.57- 0.52 131 249479.49 39.60 96.18 0.52- 0.40 140 206584.71 33.68 95.71 ------------------------------------------------------------------------------------ 5.26- 0.40 1319 411832.66 55.69 96.66 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:06:31 2018 Sorting 1319 observations 214 unique observations with > 7.00 F2/sig(F2) 1319 observations in 3 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 23 232 Total number of frames 232 Maximum number of 214 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1319 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 11 117 Total number of frames 117 1057 observations > 7.00 F2/sig(F2) 1057 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 11 117 Total number of frames 117 Removing 'redundancy=1' reflections Average redundancy: 4.9 (Out of 1057 removed 76 = 981, unique = 199) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 981 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 11 117 Total number of frames 117 199 unique data precomputed (should be 199) 199 unique data with 981 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 4.9 (Out of 981 removed 0 = 981, unique = 199) 199 unique data precomputed (should be 199) 199 unique data with 981 observations RMS deviation of equivalent data = 0.68714 Rint = 0.67242 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.65513, wR= 3.46322 Trying model 1 (ne=2, no=0)... Results: Rint= 0.72298, wR= 2.89236, Acormin=0.006, Acormax=2.109, Acor_av=0.639 F test: Probability=0.000, F= 0.816 Trying model 2 (ne=2, no=1)... Results: Rint= 0.85236, wR= 3.03592, Acormin=-0.452, Acormax=1.913, Acor_av=0.408 F test: Probability=0.000, F= 0.585 Trying model 3 (ne=4, no=0)... Results: Rint= 0.78096, wR= 2.56534, Acormin=-0.206, Acormax=2.298, Acor_av=0.457 F test: Probability=0.000, F= 0.691 Trying model 4 (ne=4, no=1)... Results: Rint= 0.84487, wR= 2.25611, Acormin=-0.748, Acormax=1.965, Acor_av=0.314 F test: Probability=0.000, F= 0.588 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96416, wR= 2.17087, Acormin=-1.214, Acormax=1.311, Acor_av=0.102 F test: Probability=0.000, F= 0.447 Trying model 6 (ne=6, no=0)... Results: Rint= 0.86166, wR= 3.08759, Acormin=-0.890, Acormax=2.647, Acor_av=0.317 F test: Probability=0.000, F= 0.558 Trying model 7 (ne=6, no=1)... Results: Rint= 0.95103, wR= 2.87488, Acormin=-1.678, Acormax=2.181, Acor_av=0.160 F test: Probability=0.000, F= 0.456 Trying model 8 (ne=6, no=3)... Results: Rint= 0.98672, wR= 2.28304, Acormin=-1.316, Acormax=1.419, Acor_av=0.065 F test: Probability=0.000, F= 0.420 Trying model 9 (ne=6, no=5)... Results: Rint= 0.99621, wR= 2.36448, Acormin=-0.547, Acormax=1.694, Acor_av=0.024 F test: Probability=0.000, F= 0.406 Trying model 10 (ne=8, no=0)... Results: Rint= 1.03254, wR= 3.78216, Acormin=-0.795, Acormax=1.921, Acor_av=0.107 F test: Probability=0.000, F= 0.380 Trying model 11 (ne=8, no=1)... Results: Rint= 1.03453, wR= 2.97025, Acormin=-0.877, Acormax=1.265, Acor_av=0.019 F test: Probability=0.000, F= 0.377 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97236, wR= 1.92793, Acormin=-0.032, Acormax=0.062, Acor_av=0.003 F test: Probability=0.000, F= 0.422 Trying model 13 (ne=8, no=5)... Results: Rint= 0.97383, wR= 2.10214, Acormin=-0.038, Acormax=0.061, Acor_av=0.003 F test: Probability=0.000, F= 0.415 Trying model 14 (ne=8, no=7)... Results: Rint= 1.01705, wR= 2.18409, Acormin=-0.042, Acormax=0.066, Acor_av=0.001 F test: Probability=0.000, F= 0.372 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.83963 There are 117 active scales (one needs to be fixed) Refinement control: frame scale #18 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 121 pars with 7381 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.68714 Using Levenberg-Marquardt: 0.00010 New wR= 0.66499 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67242 with corrections 0.64061 Rint for all data: 0.83963 with corrections 0.81729 3 observations identified as outliers and rejected Cycle 2 wR= 0.64376 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64253 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66158 with corrections 0.62863 Rint for all data: 0.83963 with corrections 0.81789 5 observations identified as outliers and rejected Cycle 3 wR= 0.62468 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62169 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64822 with corrections 0.61700 Rint for all data: 0.83963 with corrections 0.81865 4 observations identified as outliers and rejected Cycle 4 wR= 0.62012 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62055 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64306 with corrections 0.61395 Rint for all data: 0.83963 with corrections 0.81976 Final wR= 0.62055 Final frame scales: Min= 0.7841 Max= 2.6773 Final absorption correction factors: Amin= 0.5202 Amax= 1.3292 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=814.4943 max=6428878.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=117.8965 max=85440.2578 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/108 1318 reflections read from tmp file 1073 reflections are rejected (945 as outliers, 128 as groups of 1 refl) Redundancy: 1 2 3 4 5 6+ Number of groups: 0 60 26 9 1 1 Initial Chi^2= 0.61810 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88212 Current error model SIG(F2)^2 = 234.70*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 207.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 207.03*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6428879- 1288553 131 1983292.79 103.99 100.00 1288254- 692612 131 944411.70 53.59 100.00 692290- 265377 131 454009.29 46.11 100.00 264499- 179914 131 219312.63 33.84 100.00 179292- 137892 131 157207.37 24.95 100.00 137523- 105428 131 120645.33 19.57 100.00 104879- 74127 131 88661.35 15.19 100.00 73784- 6536 131 45168.32 11.23 99.24 6507- 3209 131 4445.82 3.71 72.52 3199- 814 139 2374.18 3.17 50.36 ------------------------------------------------------------------------------------ 6428879- 814 1318 399527.51 31.36 91.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 131 838766.12 69.39 97.71 1.41- 1.07 131 580948.65 46.39 96.95 1.07- 0.93 131 490371.17 35.69 96.18 0.93- 0.82 131 367100.18 28.31 87.79 0.82- 0.74 131 420313.60 29.84 93.89 0.74- 0.67 131 369118.62 26.37 93.89 0.67- 0.62 131 265751.62 22.42 91.60 0.62- 0.57 131 293921.08 21.76 83.97 0.57- 0.52 131 218490.80 18.51 88.55 0.52- 0.40 139 164826.20 15.88 89.21 ------------------------------------------------------------------------------------ 5.26- 0.40 1318 399527.51 31.36 91.96 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 131 838766.12 69.39 97.71 5.26- 1.07 262 709857.38 57.89 97.33 5.26- 0.93 393 636695.31 50.49 96.95 5.26- 0.82 524 569296.53 44.95 94.66 5.26- 0.74 655 539499.94 41.93 94.50 5.26- 0.67 786 511103.06 39.33 94.40 5.26- 0.62 917 476052.85 36.92 94.00 5.26- 0.57 1048 453286.38 35.02 92.75 5.26- 0.52 1179 427197.98 33.19 92.28 5.26- 0.40 1318 399527.51 31.36 91.96 ------------------------------------------------------------------------------------ 5.26- 0.40 1318 399527.51 31.36 91.96 Scale applied to data: s=0.155548 (maximum obs:6428878.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.819; Rsigma 0.021: data 1318 -> merged 298 With outlier rejection... Rint 0.661; Rsigma 0.023: data 1136 -> merged 298 Rejected total: 182, method kkm 176, method Blessing 6 Completeness direct cell (a, b, c) = (5.273, 5.273, 5.273), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404395, 5.272666 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 6.20 100.00 93 1.46 - 1.12 15 15 8.67 100.00 130 1.08 - 0.96 15 15 7.60 100.00 114 0.96 - 0.86 15 15 6.67 100.00 100 0.86 - 0.79 15 15 6.00 100.00 90 0.79 - 0.73 15 15 5.47 100.00 82 0.73 - 0.69 15 15 4.47 100.00 67 0.69 - 0.65 15 15 4.67 100.00 70 0.65 - 0.63 15 15 2.87 100.00 43 0.63 - 0.60 21 21 2.86 100.00 60 --------------------------------------------------------------- 5.91 - 0.60 156 156 5.44 100.00 849 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:06:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918125 5.917761 5.917587 60.0724 90.0401 59.9691 1136 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 550 614 550 589 857 764 777 1136 N (int>3sigma) = 0 514 614 514 547 821 701 707 1041 Mean intensity = 0.0 44.4 24.3 44.4 53.1 37.2 55.1 51.9 53.2 Mean int/sigma = 0.0 26.5 25.1 26.7 28.8 26.1 30.1 29.3 29.3 Lattice type: P chosen Volume: 146.59 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.915 5.917 5.918 89.96 60.02 60.01 Niggli form: a.a = 34.989 b.b = 35.016 c.c = 35.020 b.c = 0.021 a.c = 17.493 a.b = 17.494 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.091 CUBIC F-lattice R(int) = 0.175 [ 984] Vol = 586.3 Cell: 8.366 8.372 8.371 89.91 90.00 89.99 Volume: 586.34 Matrix: 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.037 RHOMBOHEDRAL R-lattice R(int) = 0.163 [ 721] Vol = 439.8 Cell: 5.915 5.917 14.505 90.06 90.00 119.99 Volume: 439.76 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.037 RHOMBOHEDRAL R-lattice R(int) = 0.155 [ 212] Vol = 439.8 Trigonal Cell: 5.915 5.917 14.505 90.06 90.00 119.99 Volume: 439.76 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.140 [ 760] Vol = 293.2 Cell: 5.918 5.918 8.371 89.94 89.94 89.96 Volume: 293.17 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.139 [ 765] Vol = 293.2 Cell: 5.918 5.918 8.371 89.94 89.94 89.96 Volume: 293.17 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.005 ORTHORHOMBIC I-lattice R(int) = 0.135 [ 709] Vol = 293.2 Cell: 5.915 8.366 5.924 89.99 89.99 90.00 Volume: 293.17 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.054 MONOCLINIC I-lattice R(int) = 0.115 [ 555] Vol = 293.2 Cell: 5.918 5.918 8.371 90.06 90.06 89.96 Volume: 293.17 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.005 MONOCLINIC I-lattice R(int) = 0.119 [ 459] Vol = 293.2 Cell: 5.915 8.366 5.924 90.01 90.01 90.00 Volume: 293.17 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.002 MONOCLINIC I-lattice R(int) = 0.129 [ 455] Vol = 293.2 Cell: 8.366 5.915 5.924 90.01 90.01 90.00 Volume: 293.17 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.095 [ 232] Vol = 146.6 Cell: 5.915 5.917 5.918 89.96 60.02 60.01 Volume: 146.59 Matrix: 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 614 0 767 770 1136 N (int>3sigma) = 0 0 0 0 614 0 705 703 1041 Mean intensity = 0.0 0.0 0.0 0.0 24.3 0.0 53.7 54.6 53.2 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 29.5 29.9 29.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.047 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 87 257 N I>3s 15 15 69 257 0.7 0.7 0.6 27.3 6.5 6.5 4.1 30.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 917 Fd-3m 1 1 227 C N N N N 37 2284 0.180 954 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366183 8.372040 8.371302 89.9132 89.9968 89.9948 ZERR 1.00 0.000388 0.002215 0.005019 0.0034 0.0164 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3519814- 732362 184 161 29 5.6 987752.50 61.24 0.590 0.525 725864- 537833 151 136 29 4.7 606276.38 42.91 0.781 0.616 537680- 428408 143 128 29 4.4 425264.10 38.86 0.803 0.788 426412- 314565 179 143 29 4.9 231351.61 23.61 0.784 0.744 308686- 224097 141 104 29 3.6 151054.35 20.77 0.562 0.568 223046- 132755 168 144 29 5.0 145770.84 22.18 0.492 0.501 130323- 93110 117 101 29 3.5 108174.54 16.12 0.308 0.263 92888- 71728 100 92 29 3.2 78539.94 13.32 0.545 0.374 71338- 46514 64 60 29 2.1 61082.75 11.78 0.542 0.490 45638- 1701 71 67 37 1.8 14035.39 5.06 0.640 0.647 ------------------------------------------------------------------------------------------- 3519814- 1701 1318 1136 298 3.8 341950.81 29.31 0.661 0.592 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 237 208 29 7.2 580389.82 55.27 0.669 0.640 0.013 1.12-0.87 242 215 29 7.4 410494.43 31.78 0.752 0.711 0.021 0.86-0.75 191 169 29 5.8 365793.60 27.32 0.589 0.535 0.025 0.74-0.67 159 134 29 4.6 325730.68 25.71 0.685 0.618 0.025 0.66-0.61 121 96 31 3.1 136969.24 15.22 0.620 0.579 0.043 0.61-0.57 112 85 30 2.8 262933.98 20.70 0.468 0.407 0.031 0.56-0.53 91 78 31 2.5 175692.91 16.76 0.651 0.567 0.038 0.53-0.49 79 70 29 2.4 136089.33 13.80 0.668 0.622 0.044 0.49-0.46 49 44 29 1.5 216941.41 18.74 0.503 0.422 0.035 0.46-0.40 37 37 32 1.2 155068.77 15.97 0.799 0.799 0.039 ------------------------------------------------------------------------------------------------------ inf-0.40 1318 1136 298 3.8 341950.81 29.31 0.661 0.592 0.023 inf-0.60 986 849 156 5.4 395903.64 33.54 0.672 0.615 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 208 29 29 100.0 7.2 580389.82 169.99 0.669 0.006 1.12-0.87 215 29 29 100.0 7.4 410494.43 102.00 0.752 0.010 0.86-0.75 169 29 29 100.0 5.8 365793.60 74.55 0.589 0.013 0.74-0.67 134 29 29 100.0 4.6 325730.68 68.76 0.685 0.015 0.66-0.61 96 31 31 100.0 3.1 136969.24 32.33 0.620 0.030 0.61-0.57 85 35 30 85.7 2.8 262933.98 39.96 0.468 0.021 0.56-0.53 78 34 31 91.2 2.5 175692.91 34.91 0.651 0.029 0.53-0.49 70 46 29 63.0 2.4 136089.33 26.64 0.668 0.033 0.49-0.46 44 57 29 50.9 1.5 216941.41 27.49 0.503 0.023 0.46-0.40 37 139 32 23.0 1.2 155068.77 18.39 0.799 0.038 -------------------------------------------------------------------------------------------- inf-0.40 1136 458 298 65.1 3.8 341950.81 81.06 0.661 0.015 inf-0.60 849 156 156 100.0 5.4 395903.64 98.37 0.672 0.012 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.024786 -0.079542 0.015541 ( 0.000010 0.000009 0.000008 ) -0.072533 -0.028953 -0.032903 ( 0.000011 0.000011 0.000008 ) 0.036229 -0.003565 -0.076517 ( 0.000008 0.000008 0.000006 ) M - matrix: 0.007188 -0.000001 -0.000000 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007178 -0.000011 ( 0.000001 0.000002 0.000001 ) -0.000000 -0.000011 0.007179 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.024786 -0.079542 0.015541 ( 0.000010 0.000009 0.000008 ) -0.072533 -0.028953 -0.032903 ( 0.000011 0.000011 0.000008 ) 0.036229 -0.003565 -0.076517 ( 0.000008 0.000008 0.000006 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3662(10) 8.3721(9) 8.3714(7) 89.914(8) 89.997(8) 89.995(9) V = 586.35(11) unit cell: 8.3699(2) 8.3699(2) 8.3699(2) 90.0 90.0 90.0 V = 586.35(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.842) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.842) Run 3 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.842) PROFFIT INFO: signal sum: min=256.0000 max=20754984.0000 PROFFIT INFO: signal sum lp corr: min=585.5218 max=2944240.9465 PROFFIT INFO: background sum: min=1061.0000 max=15205.0000 PROFFIT INFO: background sum sig2: min=607.0000 max=7484.0000 PROFFIT INFO: num of signal pixels: min=55 max=496 PROFFIT INFO: Inet: min=936.8349 max=4710785.5000 PROFFIT INFO: sig(Inet): min=96.9086 max=47420.0703 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=229.29 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 16 88 244 544 596 1000 1726 2388 2638 Percent 0.0 0.0 0.6 3.3 9.2 20.6 22.6 37.9 65.4 90.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1319 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1319 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4710786- 1280771 131 2014368.86 126.43 100.00 1273872- 772396 131 986431.54 110.04 100.00 771621- 284659 131 490270.71 94.72 100.00 283576- 182599 131 219439.66 74.34 100.00 181919- 143303 131 163150.96 53.36 100.00 142478- 107378 131 121303.55 38.67 100.00 107377- 81765 131 93569.66 31.15 100.00 81732- 6335 131 50786.35 21.91 100.00 6321- 3428 131 4581.49 5.62 98.47 3424- 937 140 2543.00 4.17 70.00 ------------------------------------------------------------------------------------ 4710786- 937 1319 411832.66 55.69 96.66 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 131 754763.60 89.22 100.00 1.39- 1.09 131 841158.83 72.06 100.00 1.09- 0.96 131 391472.98 68.02 98.47 0.96- 0.85 131 466059.85 68.65 96.18 0.85- 0.80 131 474397.30 68.77 100.00 0.80- 0.73 131 269373.46 42.93 100.00 0.73- 0.70 131 248374.07 39.88 87.79 0.70- 0.65 131 331726.25 48.90 95.42 0.65- 0.62 131 181440.57 30.42 90.84 0.62- 0.58 140 175777.26 29.84 97.86 ------------------------------------------------------------------------------------ 4.82- 0.58 1319 411832.66 55.69 96.66 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:06:32 2018 Sorting 1319 observations 81 unique observations with > 7.00 F2/sig(F2) 1319 observations in 3 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 23 232 Total number of frames 232 Maximum number of 81 frame scales suggested for reliable scaling Glued frame scales: 3 frame = 1 scale 1319 observations in 3 runs Run # start # end # total # 1 0 36 37 2 0 32 70 3 0 7 78 Total number of frames 78 1057 observations > 7.00 F2/sig(F2) 1057 observations in 3 runs Run # start # end # total # 1 0 36 37 2 0 32 70 3 0 7 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 12.1 (Out of 1057 removed 5 = 1052, unique = 87) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1052 observations in 3 runs Run # start # end # total # 1 0 36 37 2 0 32 70 3 0 7 78 Total number of frames 78 87 unique data precomputed (should be 87) 87 unique data with 1052 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 12.1 (Out of 1052 removed 0 = 1052, unique = 87) 87 unique data precomputed (should be 87) 87 unique data with 1052 observations RMS deviation of equivalent data = 0.12915 Rint = 0.09802 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.09667, wR= 0.12758 Trying model 1 (ne=2, no=0)... Results: Rint= 0.05848, wR= 0.07617, Acormin=0.784, Acormax=1.285, Acor_av=0.990 F test: Probability=1.000, F= 2.718 Trying model 2 (ne=2, no=1)... Results: Rint= 0.05927, wR= 0.07478, Acormin=0.749, Acormax=1.277, Acor_av=0.967 F test: Probability=0.000, F= 0.970 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04302, wR= 0.05674, Acormin=0.741, Acormax=1.363, Acor_av=0.954 F test: Probability=1.000, F= 1.831 Trying model 4 (ne=4, no=1)... Results: Rint= 0.03701, wR= 0.04931, Acormin=0.696, Acormax=1.339, Acor_av=0.919 F test: Probability=1.000, F= 1.347 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03399, wR= 0.04444, Acormin=0.668, Acormax=1.340, Acor_av=0.924 F test: Probability=0.994, F= 1.177 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04106, wR= 0.05448, Acormin=0.739, Acormax=1.355, Acor_av=0.949 F test: Probability=0.000, F= 0.683 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03471, wR= 0.04782, Acormin=0.696, Acormax=1.342, Acor_av=0.912 F test: Probability=0.000, F= 0.953 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03145, wR= 0.04141, Acormin=0.670, Acormax=1.361, Acor_av=0.941 F test: Probability=0.985, F= 1.152 Trying model 9 (ne=6, no=5)... Results: Rint= 0.02797, wR= 0.03537, Acormin=0.634, Acormax=1.292, Acor_av=0.902 F test: Probability=1.000, F= 1.249 Trying model 10 (ne=8, no=0)... Results: Rint= 0.03674, wR= 0.05019, Acormin=0.707, Acormax=1.318, Acor_av=0.928 F test: Probability=0.000, F= 0.582 Trying model 11 (ne=8, no=1)... Results: Rint= 0.02940, wR= 0.04141, Acormin=0.654, Acormax=1.339, Acor_av=0.861 F test: Probability=0.000, F= 0.906 Trying model 12 (ne=8, no=3)... Results: Rint= 0.02723, wR= 0.03694, Acormin=0.639, Acormax=1.266, Acor_av=0.877 F test: Probability=0.760, F= 1.048 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02225, wR= 0.03004, Acormin=0.679, Acormax=1.322, Acor_av=0.907 F test: Probability=1.000, F= 1.551 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02124, wR= 0.02874, Acormin=0.681, Acormax=1.322, Acor_av=0.914 F test: Probability=0.871, F= 1.079 Final absorption model (ne=8, no=5): Rint= 0.02225, Acormin=0.679, Acormax=1.322, Acor_av=0.907 Combined refinement in use Rint: 0.09816 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #24 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 5 (65 parameters) Refinement control: 142 pars with 10153 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.12915 Using Levenberg-Marquardt: 0.00010 New wR= 0.02509 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09802 with corrections 0.01987 Rint for all data: 0.09816 with corrections 0.02011 1 observations identified as outliers and rejected Cycle 2 wR= 0.02517 Using Levenberg-Marquardt: 0.00001 New wR= 0.02440 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09787 with corrections 0.01888 Rint for all data: 0.09816 with corrections 0.01908 1 observations identified as outliers and rejected Cycle 3 wR= 0.02387 Using Levenberg-Marquardt: 0.00000 New wR= 0.02362 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09783 with corrections 0.01878 Rint for all data: 0.09816 with corrections 0.01902 0 observations identified as outliers and rejected Cycle 4 wR= 0.02362 Using Levenberg-Marquardt: 0.00000 New wR= 0.02353 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09783 with corrections 0.01871 Rint for all data: 0.09816 with corrections 0.01894 0 observations identified as outliers and rejected Cycle 5 wR= 0.02353 Using Levenberg-Marquardt: 0.00000 New wR= 0.02348 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.09783 with corrections 0.01865 Rint for all data: 0.09816 with corrections 0.01888 0 observations identified as outliers and rejected Final wR= 0.02348 Final frame scales: Min= 0.8447 Max= 1.1220 Final absorption correction factors: Amin= 0.6699 Amax= 1.2603 PROFFIT INFO: Inet (after scale3 abspack): min=882.6934 max=4507902.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=109.1448 max=46298.7695 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1319 reflections read from tmp file 49 reflections are rejected (46 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 7 4 4 4 4 10 65 Initial Chi^2= 0.28677 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.57839 Current error model SIG(F2)^2 = 125.80*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 198.56*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 198.56*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4507902- 1281110 131 1989387.42 110.69 100.00 1273647- 749061 131 970377.11 51.10 100.00 748480- 292330 131 486263.54 49.63 100.00 292221- 181842 131 217846.10 34.90 100.00 181563- 146765 131 163286.10 25.05 100.00 146574- 104724 131 118416.79 17.89 100.00 104489- 83592 131 94505.99 15.05 100.00 83571- 6124 131 51494.32 10.82 100.00 6032- 3315 131 4457.13 3.72 78.63 3314- 883 140 2554.62 3.25 52.86 ------------------------------------------------------------------------------------ 4507902- 883 1319 407079.73 32.01 92.87 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 131 749099.86 72.70 100.00 1.39- 1.09 131 831382.38 57.83 99.24 1.09- 0.96 131 388353.38 33.72 96.18 0.96- 0.85 131 462946.89 32.93 93.13 0.85- 0.80 131 469232.36 32.30 97.71 0.80- 0.73 131 265081.64 20.51 96.18 0.73- 0.70 131 244151.06 19.10 81.68 0.70- 0.65 131 325901.24 23.07 91.60 0.65- 0.62 131 177388.62 14.73 83.21 0.62- 0.58 140 173319.72 14.46 90.00 ------------------------------------------------------------------------------------ 4.82- 0.58 1319 407079.73 32.01 92.87 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 131 749099.86 72.70 100.00 4.82- 1.09 262 790241.12 65.26 99.62 4.82- 0.96 393 656278.54 54.75 98.47 4.82- 0.85 524 607945.63 49.29 97.14 4.82- 0.80 655 580202.97 45.89 97.25 4.82- 0.73 786 527682.75 41.66 97.07 4.82- 0.70 917 487178.22 38.44 94.87 4.82- 0.65 1048 467018.60 36.52 94.47 4.82- 0.62 1179 434837.49 34.10 93.21 4.82- 0.58 1319 407079.73 32.01 92.87 ------------------------------------------------------------------------------------ 4.82- 0.58 1319 407079.73 32.01 92.87 Scale applied to data: s=0.221832 (maximum obs:4507902.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.019; Rsigma 0.020: data 1319 -> merged 108 With outlier rejection... Rint 0.017; Rsigma 0.021: data 1310 -> merged 108 Rejected total: 9, method kkm 8, method Blessing 1 Completeness direct cell (a, b, c) = (8.370, 8.370, 8.370), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586009, 4.832350 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 6.50 100.00 65 1.61 - 1.21 10 10 11.70 100.00 117 1.17 - 1.01 10 10 15.40 100.00 154 0.99 - 0.89 10 10 15.10 100.00 151 0.88 - 0.81 10 10 14.70 100.00 147 0.81 - 0.74 10 10 12.90 100.00 129 0.73 - 0.71 10 10 13.90 100.00 139 0.70 - 0.66 10 10 12.50 100.00 125 0.66 - 0.64 10 10 10.50 100.00 105 0.63 - 0.60 10 10 10.70 100.00 107 --------------------------------------------------------------- 5.91 - 0.60 100 100 12.39 100.00 1239 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:06:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918125 5.917761 5.917587 60.0724 90.0401 59.9691 1136 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.31 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 550 614 550 589 857 764 777 1136 N (int>3sigma) = 0 514 614 514 547 821 701 707 1041 Mean intensity = 0.0 44.4 24.3 44.4 53.1 37.2 55.1 51.9 53.2 Mean int/sigma = 0.0 26.5 25.1 26.7 28.8 26.1 30.1 29.3 29.3 Lattice type: P chosen Volume: 146.59 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.915 5.917 5.918 89.96 60.02 60.01 Niggli form: a.a = 34.989 b.b = 35.016 c.c = 35.020 b.c = 0.021 a.c = 17.493 a.b = 17.494 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.091 CUBIC F-lattice R(int) = 0.175 [ 984] Vol = 586.3 Cell: 8.366 8.372 8.371 89.91 90.00 89.99 Volume: 586.34 Matrix: 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.037 RHOMBOHEDRAL R-lattice R(int) = 0.163 [ 721] Vol = 439.8 Cell: 5.915 5.917 14.505 90.06 90.00 119.99 Volume: 439.76 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.037 RHOMBOHEDRAL R-lattice R(int) = 0.155 [ 212] Vol = 439.8 Trigonal Cell: 5.915 5.917 14.505 90.06 90.00 119.99 Volume: 439.76 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.140 [ 760] Vol = 293.2 Cell: 5.918 5.918 8.371 89.94 89.94 89.96 Volume: 293.17 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.139 [ 765] Vol = 293.2 Cell: 5.918 5.918 8.371 89.94 89.94 89.96 Volume: 293.17 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.005 ORTHORHOMBIC I-lattice R(int) = 0.135 [ 709] Vol = 293.2 Cell: 5.915 8.366 5.924 89.99 89.99 90.00 Volume: 293.17 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.054 MONOCLINIC I-lattice R(int) = 0.115 [ 555] Vol = 293.2 Cell: 5.918 5.918 8.371 90.06 90.06 89.96 Volume: 293.17 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.005 MONOCLINIC I-lattice R(int) = 0.119 [ 459] Vol = 293.2 Cell: 5.915 8.366 5.924 90.01 90.01 90.00 Volume: 293.17 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.002 MONOCLINIC I-lattice R(int) = 0.129 [ 455] Vol = 293.2 Cell: 8.366 5.915 5.924 90.01 90.01 90.00 Volume: 293.17 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.095 [ 232] Vol = 146.6 Cell: 5.915 5.917 5.918 89.96 60.02 60.01 Volume: 146.59 Matrix: 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 614 0 767 770 1136 N (int>3sigma) = 0 0 0 0 614 0 705 703 1041 Mean intensity = 0.0 0.0 0.0 0.0 24.3 0.0 53.7 54.6 53.2 Mean int/sigma = 0.0 0.0 0.0 0.0 25.1 0.0 29.5 29.9 29.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.047 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 87 257 N I>3s 15 15 69 257 0.7 0.7 0.6 27.3 6.5 6.5 4.1 30.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 917 Fd-3m 1 1 227 C N N N N 37 2284 0.180 954 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.366183 8.372040 8.371302 89.9132 89.9968 89.9948 ZERR 1.00 0.000388 0.002215 0.005019 0.0034 0.0164 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4322764- 622057 295 290 27 10.7 1373047.18 74.10 0.014 0.016 606962- 126932 398 395 27 14.6 238116.29 34.52 0.022 0.026 126926- 11626 331 331 27 12.3 88801.30 14.46 0.033 0.039 8842- 2176 295 294 27 10.9 3745.71 3.56 0.142 0.169 ------------------------------------------------------------------------------------------- 4322764- 2176 1319 1310 108 12.1 399033.65 31.27 0.017 0.019 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 316 308 27 11.4 688035.47 57.84 0.016 0.016 0.012 1.01-0.78 380 380 27 14.1 413703.90 30.23 0.014 0.016 0.020 0.78-0.65 381 380 29 13.1 279574.26 20.51 0.019 0.022 0.030 0.65-0.59 242 242 25 9.7 195758.10 15.97 0.031 0.034 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 1319 1310 108 12.1 399033.65 31.27 0.017 0.019 0.021 inf-0.60 1246 1237 99 12.5 414685.75 32.35 0.017 0.018 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 308 27 27 100.0 11.4 688035.47 206.82 0.016 0.004 1.01-0.78 380 27 27 100.0 14.1 413703.90 120.38 0.014 0.006 0.78-0.65 380 29 29 100.0 13.1 279574.26 78.44 0.019 0.009 0.65-0.59 242 26 25 96.2 9.7 195758.10 55.59 0.031 0.015 -------------------------------------------------------------------------------------------- inf-0.59 1310 109 108 99.1 12.1 399033.65 116.57 0.017 0.006 inf-0.60 1237 99 99 100.0 12.5 414685.75 120.96 0.017 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:13:22 2018) ID: 2932; threads 39; handles 878; mem 518368.00 (1237820.00)kB; time: 1w 4d 23h 18m 53s MEMORY INFO: Memory PF:245.0, Ph:425.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.2,peak PF: 697.1, WS: 297.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:246.0, Ph:425.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 697.1, WS: 299.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:13:22 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000019 0.000015 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000022 0.000017 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000017 0.000013 0.000012 ) 5.91502 ( 0.00105 ) 5.91640 ( 0.00106 ) 5.92265 ( 0.00079 ) 60.05206 ( 0.01630 ) 89.98756 ( 0.01254 ) 60.01743 ( 0.01869 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:13:22 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000019 0.000015 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000022 0.000017 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000017 0.000013 0.000012 ) M - matrix: 0.021566 -0.014381 0.007190 ( 0.000005 0.000004 0.000003 ) -0.014381 0.028717 -0.014337 ( 0.000004 0.000005 0.000003 ) 0.007190 -0.014337 0.021525 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9150(11) 5.9164(11) 5.9227(8) 60.052(16) 89.988(13) 60.017(19) V = 146.73(4) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.977 ( 0.156) | 1.302 ( 0.737) | 1.291 ( 0.803) | 1.32- 1.09 | 44 | 1.063 ( 0.112) | 1.087 ( 0.140) | 1.156 ( 0.505) | 1.09- 0.96 | 44 | 1.060 ( 0.106) | 1.078 ( 0.148) | 1.126 ( 0.473) | 0.94- 0.84 | 44 | 1.078 ( 0.105) | 1.066 ( 0.134) | 1.141 ( 0.405) | 0.84- 0.81 | 44 | 1.110 ( 0.099) | 1.024 ( 0.124) | 1.354 ( 0.482) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.092 ( 0.076) | 0.948 ( 0.113) | 1.416 ( 0.479) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.882 ( 0.071) | 1.412 ( 0.492) | 0.67- 0.63 | 44 | 1.072 ( 0.065) | 0.865 ( 0.062) | 1.474 ( 0.592) | 0.63- 0.59 | 45 | 1.009 ( 0.080) | 0.806 ( 0.036) | 1.283 ( 0.494) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 441 | 1.063 ( 0.106) | 1.004 ( 0.290) | 1.296 ( 0.544) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb PROFFITPEAK info: 605 peaks in the peak location table UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) UB - matrix: -0.069998 0.031096 0.089010 ( 0.000107 0.000069 0.000155 ) -0.068891 -0.065559 -0.010371 ( 0.000065 0.000042 0.000094 ) 0.109057 -0.152850 0.116029 ( 0.000086 0.000055 0.000125 ) M - matrix: 0.021539 -0.014330 0.007138 ( 0.000026 0.000016 0.000023 ) -0.014330 0.028628 -0.014287 ( 0.000016 0.000018 0.000022 ) 0.007138 -0.014287 0.021493 ( 0.000023 0.000022 0.000040 ) unit cell: 5.918(4) 5.924(4) 5.919(6) 60.06(9) 89.95(7) 59.97(7) V = 146.8(2) UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) UB - matrix: -0.069998 0.031096 0.089010 ( 0.000107 0.000069 0.000155 ) -0.068891 -0.065559 -0.010371 ( 0.000065 0.000042 0.000094 ) 0.109057 -0.152850 0.116029 ( 0.000086 0.000055 0.000125 ) M - matrix: 0.021539 -0.014330 0.007138 ( 0.000026 0.000016 0.000023 ) -0.014330 0.028628 -0.014287 ( 0.000016 0.000018 0.000022 ) 0.007138 -0.014287 0.021493 ( 0.000023 0.000022 0.000040 ) unit cell: 5.918(4) 5.924(4) 5.919(6) 60.06(9) 89.95(7) 59.97(7) V = 146.8(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.070120 0.031123 0.088933 ( 0.000107 0.000068 0.000155 ) -0.068747 -0.065783 -0.010380 ( 0.000062 0.000040 0.000090 ) 0.108929 -0.152669 0.116039 ( 0.000091 0.000058 0.000132 ) M - matrix: 0.021508 -0.014290 0.007118 ( 0.000026 0.000017 0.000024 ) -0.014290 0.028604 -0.014265 ( 0.000017 0.000019 0.000023 ) 0.007118 -0.014265 0.021482 ( 0.000024 0.000023 0.000041 ) UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) unit cell: 5.917(4) 5.920(4) 5.917(6) 60.08(9) 89.96(7) 60.02(7) V = 146.8(2) UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) UB - matrix: -0.070120 0.031123 0.088933 ( 0.000107 0.000068 0.000155 ) -0.068747 -0.065783 -0.010380 ( 0.000062 0.000040 0.000090 ) 0.108929 -0.152669 0.116039 ( 0.000091 0.000058 0.000132 ) M - matrix: 0.021508 -0.014290 0.007118 ( 0.000026 0.000017 0.000024 ) -0.014290 0.028604 -0.014265 ( 0.000017 0.000019 0.000023 ) 0.007118 -0.014265 0.021482 ( 0.000024 0.000023 0.000041 ) unit cell: 5.917(4) 5.920(4) 5.917(6) 60.08(9) 89.96(7) 60.02(7) V = 146.8(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.070120 0.031123 0.088933 ( 0.000107 0.000068 0.000155 ) -0.068747 -0.065783 -0.010380 ( 0.000062 0.000040 0.000090 ) 0.108929 -0.152669 0.116039 ( 0.000091 0.000058 0.000132 ) M - matrix: 0.021508 -0.014290 0.007118 ( 0.000026 0.000017 0.000024 ) -0.014290 0.028604 -0.014265 ( 0.000017 0.000019 0.000023 ) 0.007118 -0.014265 0.021482 ( 0.000024 0.000023 0.000041 ) UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) unit cell: 5.917(4) 5.920(4) 5.917(6) 60.08(9) 89.96(7) 60.02(7) V = 146.8(2) 287 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Run 3 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 434 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070120 0.031123 0.088933 ( 0.000107 0.000068 0.000155 ) -0.068747 -0.065783 -0.010380 ( 0.000062 0.000040 0.000090 ) 0.108929 -0.152669 0.116039 ( 0.000091 0.000058 0.000132 ) M - matrix: 0.021508 -0.014290 0.007118 ( 0.000026 0.000017 0.000024 ) -0.014290 0.028604 -0.014265 ( 0.000017 0.000019 0.000023 ) 0.007118 -0.014265 0.021482 ( 0.000024 0.000023 0.000041 ) UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) unit cell: 5.917(4) 5.920(4) 5.917(6) 60.08(9) 89.96(7) 60.02(7) V = 146.8(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 280 obs out of 287 (total:287,skipped:0) (97.56%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb 3 of 218 peaks identified as outliers and rejected 215 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 215 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 215 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.47 | 22 | 0.973 ( 0.120) | 1.013 ( 0.151) | 1.011 ( 0.344) | 1.41- 1.17 | 22 | 1.078 ( 0.161) | 1.258 ( 0.615) | 1.144 ( 0.641) | 1.17- 1.02 | 22 | 1.019 ( 0.089) | 1.066 ( 0.247) | 1.069 ( 0.514) | 1.01- 0.92 | 22 | 1.017 ( 0.095) | 1.026 ( 0.094) | 0.954 ( 0.367) | 0.92- 0.82 | 22 | 1.019 ( 0.089) | 0.964 ( 0.109) | 1.205 ( 0.454) | 0.81- 0.75 | 22 | 1.020 ( 0.076) | 0.959 ( 0.117) | 1.170 ( 0.483) | 0.74- 0.69 | 22 | 0.992 ( 0.041) | 0.897 ( 0.053) | 1.344 ( 0.508) | 0.69- 0.64 | 22 | 0.972 ( 0.050) | 0.858 ( 0.048) | 1.243 ( 0.439) | 0.64- 0.62 | 22 | 0.951 ( 0.038) | 0.846 ( 0.029) | 1.220 ( 0.413) | 0.62- 0.59 | 17 | 0.926 ( 0.044) | 0.813 ( 0.032) | 1.242 ( 0.486) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 215 | 0.998 ( 0.098) | 0.974 ( 0.258) | 1.158 ( 0.485) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) UB - matrix: -0.070199 0.031030 0.089104 ( 0.000056 0.000035 0.000082 ) -0.068414 -0.066130 -0.010306 ( 0.000032 0.000020 0.000047 ) 0.109030 -0.152863 0.116145 ( 0.000032 0.000020 0.000047 ) M - matrix: 0.021496 -0.014321 0.007113 ( 0.000011 0.000007 0.000010 ) -0.014321 0.028703 -0.014308 ( 0.000007 0.000007 0.000009 ) 0.007113 -0.014308 0.021536 ( 0.000010 0.000009 0.000018 ) unit cell: 5.921(2) 5.913(2) 5.910(3) 60.06(5) 89.90(4) 59.97(4) V = 146.50(11) OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 UB - matrix: -0.069971 0.031045 0.088931 ( 0.000053 0.000033 0.000077 ) -0.068681 -0.065769 -0.010285 ( 0.000020 0.000012 0.000029 ) 0.108998 -0.152753 0.116164 ( 0.000032 0.000020 0.000047 ) M - matrix: 0.021494 -0.014305 0.007145 ( 0.000011 0.000006 0.000010 ) -0.014305 0.028623 -0.014307 ( 0.000006 0.000007 0.000009 ) 0.007145 -0.014307 0.021508 ( 0.000010 0.000009 0.000018 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 5.9223(17) 5.9244(15) 5.920(3) 60.03(4) 89.98(3) 60.02(3) V = 146.98(10) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 434 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069971 0.031045 0.088931 ( 0.000053 0.000033 0.000077 ) -0.068681 -0.065769 -0.010285 ( 0.000020 0.000012 0.000029 ) 0.108998 -0.152753 0.116164 ( 0.000032 0.000020 0.000047 ) M - matrix: 0.021494 -0.014305 0.007145 ( 0.000011 0.000006 0.000010 ) -0.014305 0.028623 -0.014307 ( 0.000006 0.000007 0.000009 ) 0.007145 -0.014307 0.021508 ( 0.000010 0.000009 0.000018 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 5.9223(17) 5.9244(15) 5.920(3) 60.03(4) 89.98(3) 60.02(3) V = 146.98(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb 4 of 220 peaks identified as outliers and rejected 216 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 216 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 216 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 22 | 1.029 ( 0.307) | 1.090 ( 0.409) | 0.976 ( 0.329) | 1.48- 1.17 | 22 | 1.060 ( 0.159) | 1.226 ( 0.629) | 1.119 ( 0.590) | 1.17- 1.02 | 22 | 1.025 ( 0.081) | 1.068 ( 0.245) | 1.078 ( 0.492) | 1.02- 0.92 | 22 | 1.016 ( 0.096) | 1.026 ( 0.092) | 0.972 ( 0.384) | 0.92- 0.82 | 22 | 1.019 ( 0.094) | 0.973 ( 0.106) | 1.141 ( 0.420) | 0.82- 0.75 | 22 | 1.020 ( 0.078) | 0.951 ( 0.108) | 1.197 ( 0.472) | 0.75- 0.70 | 22 | 0.991 ( 0.044) | 0.893 ( 0.059) | 1.332 ( 0.514) | 0.69- 0.65 | 22 | 0.972 ( 0.050) | 0.866 ( 0.051) | 1.239 ( 0.441) | 0.65- 0.62 | 22 | 0.955 ( 0.039) | 0.848 ( 0.027) | 1.211 ( 0.422) | 0.62- 0.59 | 18 | 0.926 ( 0.042) | 0.812 ( 0.033) | 1.227 ( 0.477) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 216 | 1.003 ( 0.132) | 0.978 ( 0.287) | 1.148 ( 0.472) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.5 | 106 | 1.129 ( 0.140) | 1.284 ( 0.532) | 1.196 ( 0.594) | 12.5-19.2 | 106 | 1.088 ( 0.059) | 1.144 ( 0.270) | 1.214 ( 0.532) | 19.2-23.3 | 106 | 1.078 ( 0.073) | 1.111 ( 0.242) | 1.140 ( 0.424) | 23.3-27.4 | 106 | 1.047 ( 0.089) | 1.112 ( 0.354) | 1.262 ( 0.631) | 27.4-31.1 | 106 | 1.027 ( 0.089) | 1.003 ( 0.189) | 1.235 ( 0.506) | 31.1-34.0 | 106 | 0.991 ( 0.092) | 0.927 ( 0.108) | 1.230 ( 0.524) | 34.1-36.9 | 106 | 0.973 ( 0.084) | 0.898 ( 0.098) | 1.235 ( 0.494) | 36.9-39.7 | 106 | 0.963 ( 0.104) | 0.894 ( 0.172) | 1.212 ( 0.562) | 39.7-42.8 | 106 | 0.935 ( 0.094) | 0.842 ( 0.093) | 1.173 ( 0.489) | 42.8-49.9 | 108 | 0.951 ( 0.088) | 0.828 ( 0.067) | 1.161 ( 0.458) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1062 | 1.018 ( 0.112) | 1.004 ( 0.291) | 1.206 ( 0.526) | Fitted profile normalization line parameters e1 dimension: a=-0.0045 b=1.15 e2 dimension: a=-0.0099 b=1.27 e3 dimension: a=0.0024 b=0.99 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 9708196 lp-corr: 2429818 PROFFITPEAK - Finished at Tue Mar 27 14:13:38 2018 PROFFITMAIN - Started at Tue Mar 27 14:13:38 2018 OTKP changes: 1062 2 3 3 OTKP changes: 1062 2 3 3 UB - matrix: -0.070275 0.031084 0.088846 ( 0.000019 0.000014 0.000014 ) -0.068647 -0.065813 -0.010651 ( 0.000019 0.000015 0.000014 ) 0.109209 -0.153100 0.116338 ( 0.000015 0.000012 0.000011 ) M - matrix: 0.021578 -0.014386 0.007193 ( 0.000005 0.000003 0.000003 ) -0.014386 0.028737 -0.014349 ( 0.000003 0.000004 0.000003 ) 0.007193 -0.014349 0.021542 ( 0.000003 0.000003 0.000004 ) UB fit with 1062 obs out of 1062 (total:1062,skipped:0) (100.00%) unit cell: 5.9159(9) 5.9153(10) 5.9155(8) 60.067(15) 90.037(12) 59.977(17) V = 146.43(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070090 0.030691 0.088908 ( 0.000028 0.000027 0.000016 ) -0.068208 -0.066122 -0.010577 ( 0.000024 0.000024 0.000014 ) 0.109103 -0.153084 0.116039 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021468 -0.014343 0.007150 ( 0.000007 0.000006 0.000004 ) -0.014343 0.028749 -0.014336 ( 0.000006 0.000008 0.000004 ) 0.007150 -0.014336 0.021482 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9289(14) 5.9144(14) 5.9246(11) 60.03(2) 89.991(17) 59.99(2) V = 146.94(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070285 0.030887 0.088784 ( 0.000026 0.000026 0.000015 ) -0.068386 -0.066087 -0.010712 ( 0.000024 0.000023 0.000013 ) 0.109291 -0.153238 0.116308 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014399 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028803 -0.014373 ( 0.000005 0.000008 0.000004 ) 0.007204 -0.014373 0.021525 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9098(13) 5.9205(10) 60.05(2) 90.075(16) 60.00(2) V = 146.44(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.832) HKL list info: 807 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070285 0.030887 0.088784 ( 0.000026 0.000026 0.000015 ) -0.068386 -0.066087 -0.010712 ( 0.000024 0.000023 0.000013 ) 0.109291 -0.153238 0.116308 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014399 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028803 -0.014373 ( 0.000005 0.000008 0.000004 ) 0.007204 -0.014373 0.021525 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9098(13) 5.9205(10) 60.05(2) 90.075(16) 60.00(2) V = 146.44(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070285 0.030887 0.088784 ( 0.000026 0.000026 0.000015 ) -0.068386 -0.066087 -0.010712 ( 0.000024 0.000023 0.000013 ) 0.109291 -0.153238 0.116308 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021561 -0.014399 0.007204 ( 0.000007 0.000005 0.000004 ) -0.014399 0.028803 -0.014373 ( 0.000005 0.000008 0.000004 ) 0.007204 -0.014373 0.021525 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9184(13) 5.9098(13) 5.9205(10) 60.05(2) 90.075(16) 60.00(2) V = 146.44(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070404 0.031304 0.088608 ( 0.000025 0.000021 0.000026 ) -0.068598 -0.065953 -0.010295 ( 0.000031 0.000027 0.000033 ) 0.109012 -0.152740 0.116271 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021546 -0.014330 0.007143 ( 0.000007 0.000005 0.000005 ) -0.014330 0.028659 -0.014307 ( 0.000005 0.000006 0.000005 ) 0.007143 -0.014307 0.021476 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(16) 5.9212(16) 5.9243(13) 60.01(3) 89.96(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070340 0.031171 0.088809 ( 0.000023 0.000020 0.000025 ) -0.068727 -0.065865 -0.010338 ( 0.000030 0.000026 0.000032 ) 0.109134 -0.153086 0.116526 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021581 -0.014373 0.007181 ( 0.000007 0.000005 0.000005 ) -0.014373 0.028745 -0.014389 ( 0.000005 0.000006 0.000005 ) 0.007181 -0.014389 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9119(16) 5.9187(16) 5.9172(12) 59.94(2) 89.944(19) 60.00(3) V = 146.35(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.832) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070340 0.031171 0.088809 ( 0.000023 0.000020 0.000025 ) -0.068727 -0.065865 -0.010338 ( 0.000030 0.000026 0.000032 ) 0.109134 -0.153086 0.116526 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021581 -0.014373 0.007181 ( 0.000007 0.000005 0.000005 ) -0.014373 0.028745 -0.014389 ( 0.000005 0.000006 0.000005 ) 0.007181 -0.014389 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9119(16) 5.9187(16) 5.9172(12) 59.94(2) 89.944(19) 60.00(3) V = 146.35(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070340 0.031171 0.088809 ( 0.000023 0.000020 0.000025 ) -0.068727 -0.065865 -0.010338 ( 0.000030 0.000026 0.000032 ) 0.109134 -0.153086 0.116526 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021581 -0.014373 0.007181 ( 0.000007 0.000005 0.000005 ) -0.014373 0.028745 -0.014389 ( 0.000005 0.000006 0.000005 ) 0.007181 -0.014389 0.021572 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9119(16) 5.9187(16) 5.9172(12) 59.94(2) 89.944(19) 60.00(3) V = 146.35(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) UB - matrix: -0.070056 0.031030 0.089037 ( 0.000053 0.000033 0.000078 ) -0.068554 -0.065924 -0.010299 ( 0.000024 0.000015 0.000036 ) 0.109034 -0.152850 0.116156 ( 0.000036 0.000022 0.000052 ) M - matrix: 0.021496 -0.014320 0.007133 ( 0.000011 0.000007 0.000010 ) -0.014320 0.028672 -0.014313 ( 0.000007 0.000007 0.000010 ) 0.007133 -0.014313 0.021526 ( 0.000010 0.000010 0.000018 ) unit cell: 5.9224(19) 5.9188(17) 5.915(3) 60.04(4) 89.94(3) 59.98(3) V = 146.73(10) OTKP changes: 216 1 1 1 OTKP changes: 216 1 1 1 OTKP changes: 216 1 1 1 UB - matrix: -0.070095 0.030931 0.089168 ( 0.000053 0.000033 0.000077 ) -0.068801 -0.065828 -0.010415 ( 0.000021 0.000013 0.000031 ) 0.109260 -0.153087 0.116294 ( 0.000035 0.000022 0.000051 ) M - matrix: 0.021585 -0.014365 0.007173 ( 0.000011 0.000007 0.000010 ) -0.014365 0.028726 -0.014359 ( 0.000007 0.000007 0.000009 ) 0.007173 -0.014359 0.021584 ( 0.000010 0.000009 0.000018 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.9107(18) 5.9151(16) 5.910(3) 60.02(4) 89.97(3) 60.00(3) V = 146.18(10) Run 3 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.832) HKL list info: 426 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070095 0.030931 0.089168 ( 0.000053 0.000033 0.000077 ) -0.068801 -0.065828 -0.010415 ( 0.000021 0.000013 0.000031 ) 0.109260 -0.153087 0.116294 ( 0.000035 0.000022 0.000051 ) M - matrix: 0.021585 -0.014365 0.007173 ( 0.000011 0.000007 0.000010 ) -0.014365 0.028726 -0.014359 ( 0.000007 0.000007 0.000009 ) 0.007173 -0.014359 0.021584 ( 0.000010 0.000009 0.000018 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.9107(18) 5.9151(16) 5.910(3) 60.02(4) 89.97(3) 60.00(3) V = 146.18(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.070095 0.030931 0.089168 ( 0.000053 0.000033 0.000077 ) -0.068801 -0.065828 -0.010415 ( 0.000021 0.000013 0.000031 ) 0.109260 -0.153087 0.116294 ( 0.000035 0.000022 0.000051 ) M - matrix: 0.021585 -0.014365 0.007173 ( 0.000011 0.000007 0.000010 ) -0.014365 0.028726 -0.014359 ( 0.000007 0.000007 0.000009 ) 0.007173 -0.014359 0.021584 ( 0.000010 0.000009 0.000018 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.9107(18) 5.9151(16) 5.910(3) 60.02(4) 89.97(3) 60.00(3) V = 146.18(10) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070273 0.031076 0.088807 ( 0.000019 0.000014 0.000014 ) -0.068623 -0.065789 -0.010684 ( 0.000019 0.000015 0.000014 ) 0.109202 -0.153066 0.116332 ( 0.000015 0.000012 0.000011 ) M - matrix: 0.021572 -0.014384 0.007196 ( 0.000005 0.000003 0.000003 ) -0.014384 0.028723 -0.014344 ( 0.000003 0.000004 0.000003 ) 0.007196 -0.014344 0.021534 ( 0.000003 0.000003 0.000004 ) UB fit with 1062 obs out of 1062 (total:1062,skipped:0) (100.00%) unit cell: 5.9172(10) 5.9171(10) 5.9168(8) 60.072(15) 90.051(12) 59.976(17) V = 146.53(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 57 reflections under beam stop or inside a detector rejection region 9 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof 1475 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:13:41 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.832) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.832) Run 3 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.832) PROFFIT INFO: signal sum: min=237.0000 max=20672450.0000 PROFFIT INFO: signal sum lp corr: min=589.5453 max=2946648.5205 PROFFIT INFO: background sum: min=1049.0000 max=15647.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=7422.0000 PROFFIT INFO: num of signal pixels: min=52 max=539 PROFFIT INFO: Inet: min=943.2726 max=4714637.5000 PROFFIT INFO: sig(Inet): min=96.9212 max=47427.3984 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=229.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 46 136 301 331 564 967 1336 1475 Percent 0.0 0.0 0.5 3.1 9.2 20.4 22.4 38.2 65.6 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1475 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1475 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4714638- 1261946 147 1973437.25 127.39 100.00 1261218- 760378 147 970268.93 108.95 100.00 757736- 271879 147 476610.17 95.01 100.00 271523- 177233 147 212578.80 73.09 100.00 177042- 139581 147 159649.08 51.98 100.00 139530- 105963 147 119368.58 38.43 100.00 105502- 81728 147 93383.81 31.14 100.00 81663- 6099 147 49291.17 21.28 100.00 6064- 3341 147 4456.78 5.68 97.96 3337- 943 152 2500.76 4.31 71.71 ------------------------------------------------------------------------------------ 4714638- 943 1475 404786.21 55.55 96.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 147 707085.81 85.99 99.32 1.41- 1.12 147 567885.07 68.99 97.96 1.12- 0.96 147 472082.14 63.55 97.28 0.96- 0.82 147 447906.45 56.10 96.60 0.82- 0.74 147 408396.91 57.58 97.28 0.74- 0.68 147 369267.64 53.46 97.28 0.68- 0.63 147 319312.46 50.66 97.96 0.63- 0.57 147 308511.16 46.14 92.52 0.57- 0.52 147 250699.97 40.03 96.60 0.52- 0.40 152 203559.00 33.76 96.05 ------------------------------------------------------------------------------------ 5.26- 0.40 1475 404786.21 55.55 96.88 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:13:41 2018 Sorting 1475 observations 219 unique observations with > 7.00 F2/sig(F2) 1475 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 49 257 Total number of frames 257 Maximum number of 219 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1475 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 24 130 Total number of frames 130 1186 observations > 7.00 F2/sig(F2) 1186 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 24 130 Total number of frames 130 Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1186 removed 66 = 1120, unique = 210) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1120 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 24 130 Total number of frames 130 210 unique data precomputed (should be 210) 210 unique data with 1120 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.3 (Out of 1120 removed 0 = 1120, unique = 210) 210 unique data precomputed (should be 210) 210 unique data with 1120 observations RMS deviation of equivalent data = 0.69693 Rint = 0.67393 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66147, wR= 4.21314 Trying model 1 (ne=2, no=0)... Results: Rint= 0.73637, wR= 3.24802, Acormin=-0.050, Acormax=2.165, Acor_av=0.620 F test: Probability=0.000, F= 0.802 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88784, wR= 3.21479, Acormin=-0.452, Acormax=1.890, Acor_av=0.362 F test: Probability=0.000, F= 0.550 Trying model 3 (ne=4, no=0)... Results: Rint= 0.78021, wR= 2.74073, Acormin=-0.174, Acormax=2.207, Acor_av=0.475 F test: Probability=0.000, F= 0.708 Trying model 4 (ne=4, no=1)... Results: Rint= 0.87651, wR= 2.74790, Acormin=-0.526, Acormax=2.018, Acor_av=0.299 F test: Probability=0.000, F= 0.559 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96065, wR= 2.40700, Acormin=-1.147, Acormax=1.397, Acor_av=0.091 F test: Probability=0.000, F= 0.462 Trying model 6 (ne=6, no=0)... Results: Rint= 0.87372, wR= 3.16137, Acormin=-0.518, Acormax=2.783, Acor_av=0.336 F test: Probability=0.000, F= 0.556 Trying model 7 (ne=6, no=1)... Results: Rint= 0.96841, wR= 3.11339, Acormin=-0.878, Acormax=2.278, Acor_av=0.183 F test: Probability=0.000, F= 0.451 Trying model 8 (ne=6, no=3)... Results: Rint= 0.98517, wR= 3.04102, Acormin=-1.156, Acormax=1.500, Acor_av=0.063 F test: Probability=0.000, F= 0.432 Trying model 9 (ne=6, no=5)... Results: Rint= 1.00286, wR= 2.44416, Acormin=-0.480, Acormax=1.858, Acor_av=0.018 F test: Probability=0.000, F= 0.412 Trying model 10 (ne=8, no=0)... Results: Rint= 0.98574, wR= 3.17561, Acormin=-0.866, Acormax=3.125, Acor_av=0.182 F test: Probability=0.000, F= 0.428 Trying model 11 (ne=8, no=1)... Results: Rint= 1.02307, wR= 2.57829, Acormin=-1.023, Acormax=1.569, Acor_av=0.020 F test: Probability=0.000, F= 0.396 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97053, wR= 1.94982, Acormin=-0.039, Acormax=0.082, Acor_av=0.002 F test: Probability=0.000, F= 0.437 Trying model 13 (ne=8, no=5)... Results: Rint= 0.96421, wR= 1.85117, Acormin=-0.037, Acormax=0.086, Acor_av=0.003 F test: Probability=0.000, F= 0.437 Trying model 14 (ne=8, no=7)... Results: Rint= 0.99299, wR= 1.52630, Acormin=-0.043, Acormax=0.067, Acor_av=0.001 F test: Probability=0.000, F= 0.405 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.84384 There are 130 active scales (one needs to be fixed) Refinement control: frame scale #36 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 134 pars with 9045 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.69693 Using Levenberg-Marquardt: 0.00010 New wR= 0.68213 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67393 with corrections 0.65141 Rint for all data: 0.84384 with corrections 0.82657 5 observations identified as outliers and rejected Cycle 2 wR= 0.65558 Using Levenberg-Marquardt: 0.00001 New wR= 0.65217 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65887 with corrections 0.63607 Rint for all data: 0.84384 with corrections 0.82680 7 observations identified as outliers and rejected Cycle 3 wR= 0.62823 Using Levenberg-Marquardt: 0.00000 New wR= 0.63046 Using Levenberg-Marquardt: 0.00001 New wR= 0.63043 Using Levenberg-Marquardt: 0.00010 New wR= 0.63020 Using Levenberg-Marquardt: 0.00100 New wR= 0.62867 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64713 with corrections 0.63560 Rint for all data: 0.84384 with corrections 0.83256 Final wR= 0.62867 Final frame scales: Min= 1.0000 Max= 3.8147 Final absorption correction factors: Amin= 0.4848 Amax= 1.5961 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=781.0599 max=6005400.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=115.9094 max=72399.3203 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/108 1474 reflections read from tmp file 1150 reflections are rejected (1040 as outliers, 110 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 73 37 11 2 1 1 Initial Chi^2= 0.59790 Cycle 1, Chi^2= 0.91835 Current error model SIG(F2)^2 = 128.48*I_RAW + 30.71*I_BACK+(0.03813*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 0.98247 Current error model SIG(F2)^2 = 196.26*I_RAW + 0.00*I_BACK+(0.01692*)^2 Cycle 3, Chi^2= 1.00294 Current error model SIG(F2)^2 = 200.36*I_RAW + 0.00*I_BACK+(0.01411*)^2 Cycle 4, Chi^2= 0.99936 Current error model SIG(F2)^2 = 199.03*I_RAW + 0.00*I_BACK+(0.01480*)^2 Cycle 5, Chi^2= 1.00021 Current error model SIG(F2)^2 = 199.50*I_RAW + 0.00*I_BACK+(0.01459*)^2 Cycle 6, Chi^2= 0.99994 Current error model SIG(F2)^2 = 199.36*I_RAW + 0.00*I_BACK+(0.01465*)^2 Final Chi^2= 0.99994 Final error model SIG(F2)^2 = 199.36*I_RAW + 0.00*I_BACK+(0.01465*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6005401- 1243053 147 2066622.54 97.60 100.00 1237459- 645151 147 914554.18 51.24 100.00 644919- 280796 147 440963.35 46.24 100.00 280072- 186515 147 222685.53 32.74 100.00 185545- 138163 147 159340.92 23.35 100.00 137745- 98258 147 116916.44 18.11 100.00 98217- 71159 147 84661.17 14.67 100.00 71136- 6339 147 40667.45 10.95 97.96 6314- 3191 147 4195.45 3.55 72.11 3188- 781 151 2365.42 3.00 43.05 ------------------------------------------------------------------------------------ 6005401- 781 1474 404203.81 30.07 91.18 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 147 846210.50 61.87 97.28 1.41- 1.12 147 597146.18 43.52 95.24 1.07- 0.96 147 510595.75 34.87 94.56 0.96- 0.82 147 462210.74 30.06 87.07 0.82- 0.74 147 392264.74 27.26 92.52 0.74- 0.68 147 356346.89 25.66 92.52 0.68- 0.63 147 280376.73 23.16 88.44 0.63- 0.57 147 262163.60 20.74 84.35 0.57- 0.52 147 199612.87 18.48 90.48 0.52- 0.40 151 142238.36 15.49 89.40 ------------------------------------------------------------------------------------ 5.26- 0.40 1474 404203.81 30.07 91.18 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 147 846210.50 61.87 97.28 5.26- 1.12 294 721678.34 52.69 96.26 5.26- 0.96 441 651317.48 46.75 95.69 5.26- 0.82 588 604040.79 42.58 93.54 5.26- 0.74 735 561685.58 39.51 93.33 5.26- 0.68 882 527462.47 37.21 93.20 5.26- 0.63 1029 492164.51 35.20 92.52 5.26- 0.57 1176 463414.39 33.39 91.50 5.26- 0.52 1323 434103.11 31.74 91.38 5.26- 0.40 1474 404203.81 30.07 91.18 ------------------------------------------------------------------------------------ 5.26- 0.40 1474 404203.81 30.07 91.18 Scale applied to data: s=0.166517 (maximum obs:6005400.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.832; Rsigma 0.021: data 1474 -> merged 299 With outlier rejection... Rint 0.713; Rsigma 0.022: data 1312 -> merged 299 Rejected total: 162, method kkm 155, method Blessing 7 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404343, 5.271983 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 7.27 100.00 109 1.46 - 1.12 15 15 10.20 100.00 153 1.08 - 0.96 15 15 9.13 100.00 137 0.96 - 0.86 15 15 8.13 100.00 122 0.86 - 0.79 15 15 6.67 100.00 100 0.79 - 0.73 15 15 6.20 100.00 93 0.73 - 0.69 15 15 5.13 100.00 77 0.69 - 0.65 15 15 4.87 100.00 73 0.65 - 0.63 15 15 3.73 100.00 56 0.63 - 0.60 21 21 3.67 100.00 77 --------------------------------------------------------------- 5.92 - 0.60 156 156 6.39 100.00 997 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:13:42 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917237 5.917084 5.916820 60.0719 90.0512 59.9763 1312 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.43 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 639 705 640 670 992 886 901 1312 N (int>3sigma) = 0 588 705 589 623 941 809 820 1196 Mean intensity = 0.0 52.4 26.6 52.4 59.9 43.3 63.3 60.5 61.2 Mean int/sigma = 0.0 27.2 24.4 27.3 28.4 26.2 29.0 28.4 28.4 Lattice type: P chosen Volume: 146.53 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.915 5.916 5.917 89.96 60.01 60.01 Niggli form: a.a = 34.988 b.b = 35.000 c.c = 35.012 b.c = 0.026 a.c = 17.493 a.b = 17.489 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.094 CUBIC F-lattice R(int) = 0.173 [ 1160] Vol = 586.1 Cell: 8.364 8.372 8.370 89.92 89.99 90.00 Volume: 586.11 Matrix: 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.034 RHOMBOHEDRAL R-lattice R(int) = 0.167 [ 893] Vol = 439.6 Cell: 5.915 5.916 14.503 90.07 90.00 119.99 Volume: 439.59 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.034 RHOMBOHEDRAL R-lattice R(int) = 0.163 [ 262] Vol = 439.6 Trigonal Cell: 5.915 5.916 14.503 90.07 90.00 119.99 Volume: 439.59 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.154 [ 932] Vol = 293.1 Cell: 5.917 5.917 8.370 89.95 89.94 89.95 Volume: 293.06 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 933] Vol = 293.1 Cell: 5.917 5.917 8.370 89.94 89.95 89.95 Volume: 293.06 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.136 [ 880] Vol = 293.1 Cell: 5.915 8.364 5.923 89.99 89.99 90.00 Volume: 293.06 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.134 [ 717] Vol = 293.1 Cell: 5.917 5.917 8.370 90.05 90.06 89.95 Volume: 293.06 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.013 MONOCLINIC I-lattice R(int) = 0.122 [ 618] Vol = 293.1 Cell: 5.915 8.364 5.923 90.01 90.01 90.00 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.005 MONOCLINIC I-lattice R(int) = 0.128 [ 598] Vol = 293.1 Cell: 8.364 5.915 5.923 90.01 90.01 90.00 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.100 [ 356] Vol = 146.5 Cell: 5.915 5.916 5.917 89.96 60.01 60.01 Volume: 146.53 Matrix: 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 705 0 882 894 1312 N (int>3sigma) = 0 0 0 0 705 0 807 815 1196 Mean intensity = 0.0 0.0 0.0 0.0 26.6 0.0 62.1 61.8 61.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 28.5 28.2 28.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.068 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 16 16 99 288 N I>3s 16 16 73 288 0.9 0.9 0.7 31.3 6.9 6.9 4.1 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.173 1081 Fd-3m 1 1 227 C N N N N 37 2284 0.176 1118 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364202 8.371680 8.370381 89.9193 89.9900 89.9960 ZERR 1.00 0.000355 0.002080 0.004573 0.0026 0.0151 0.0019 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3163488- 714389 210 190 29 6.6 1099746.39 55.86 0.639 0.614 703514- 549723 195 183 29 6.3 581179.88 43.02 0.841 0.794 533861- 402880 168 153 29 5.3 374227.89 29.49 0.928 0.831 401131- 311917 179 146 29 5.0 287465.04 25.60 0.778 0.699 309149- 220736 156 121 29 4.2 161267.34 22.39 0.561 0.570 211843- 132773 187 167 29 5.8 147044.85 20.81 0.564 0.602 123853- 86465 131 120 29 4.1 103092.56 16.78 0.378 0.339 84802- 66369 89 81 29 2.8 73790.82 13.40 0.415 0.284 66275- 43307 79 74 29 2.6 57775.66 11.70 0.610 0.451 41482- 1402 80 77 38 2.0 16402.39 5.40 0.823 0.808 ------------------------------------------------------------------------------------------- 3163488- 1402 1474 1312 299 4.4 367752.20 28.43 0.713 0.662 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.15 277 246 29 8.5 678282.70 50.23 0.719 0.754 0.014 1.12-0.87 272 258 29 8.9 471621.97 32.76 0.848 0.847 0.020 0.86-0.75 213 193 29 6.7 333363.13 24.84 0.597 0.572 0.028 0.74-0.67 176 147 29 5.1 321506.97 24.80 0.668 0.582 0.026 0.66-0.61 137 122 32 3.8 170814.67 17.48 0.801 0.769 0.036 0.61-0.57 118 102 29 3.5 262526.94 20.66 0.508 0.468 0.031 0.56-0.53 103 89 31 2.9 154754.91 16.57 0.630 0.541 0.039 0.53-0.49 92 76 31 2.5 115876.69 13.55 0.499 0.424 0.045 0.49-0.46 51 44 29 1.5 168848.60 17.61 0.373 0.369 0.038 0.46-0.40 35 35 31 1.1 135084.82 15.25 0.698 0.698 0.041 ------------------------------------------------------------------------------------------------------ inf-0.40 1474 1312 299 4.4 367752.20 28.43 0.713 0.662 0.022 inf-0.60 1110 997 156 6.4 433355.35 32.20 0.729 0.707 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.15 246 29 29 100.0 8.5 678282.70 176.48 0.719 0.006 1.12-0.87 258 29 29 100.0 8.9 471621.97 123.34 0.848 0.009 0.86-0.75 193 29 29 100.0 6.7 333363.13 75.91 0.597 0.013 0.74-0.67 147 29 29 100.0 5.1 321506.97 67.09 0.668 0.015 0.66-0.61 122 32 32 100.0 3.8 170814.67 44.85 0.801 0.023 0.61-0.57 102 34 29 85.3 3.5 262526.94 46.32 0.508 0.019 0.56-0.53 89 34 31 91.2 2.9 154754.91 36.06 0.630 0.026 0.53-0.49 76 48 31 64.6 2.5 115876.69 24.81 0.499 0.033 0.49-0.46 44 60 29 48.3 1.5 168848.60 24.46 0.373 0.027 0.46-0.40 35 140 31 22.1 1.1 135084.82 17.03 0.698 0.041 -------------------------------------------------------------------------------------------- inf-0.40 1312 464 299 64.4 4.4 367752.20 88.96 0.713 0.014 inf-0.60 997 156 156 100.0 6.4 433355.35 107.26 0.729 0.011 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 2.0 -1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 1.0 0.0 -1.0 -1.0 2.0 -1.0 No constraint UB - matrix: 0.024806 -0.079539 0.015538 ( 0.000010 0.000009 0.000007 ) -0.072548 -0.028969 -0.032894 ( 0.000010 0.000010 0.000007 ) 0.036234 -0.003565 -0.076533 ( 0.000008 0.000008 0.000006 ) M - matrix: 0.007191 -0.000001 -0.000001 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007178 -0.000010 ( 0.000001 0.000002 0.000001 ) -0.000001 -0.000010 0.007181 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.024806 -0.079539 0.015538 ( 0.000010 0.000009 0.000007 ) -0.072548 -0.028969 -0.032894 ( 0.000010 0.000010 0.000007 ) 0.036234 -0.003565 -0.076533 ( 0.000008 0.000008 0.000006 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3642(9) 8.3717(9) 8.3704(7) 89.920(8) 89.990(7) 89.996(9) V = 586.12(10) unit cell: 8.3688(2) 8.3688(2) 8.3688(2) 90.0 90.0 90.0 V = 586.12(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.832) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.832) Run 3 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.832) PROFFIT INFO: signal sum: min=237.0000 max=20672450.0000 PROFFIT INFO: signal sum lp corr: min=589.5453 max=2946648.5205 PROFFIT INFO: background sum: min=1049.0000 max=15647.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=7422.0000 PROFFIT INFO: num of signal pixels: min=52 max=539 PROFFIT INFO: Inet: min=943.2726 max=4714637.5000 PROFFIT INFO: sig(Inet): min=96.9212 max=47427.3984 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=229.35 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 16 92 272 602 662 1128 1934 2672 2950 Percent 0.0 0.0 0.5 3.1 9.2 20.4 22.4 38.2 65.6 90.6 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1475 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1475 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4714638- 1261946 147 1973437.25 127.39 100.00 1261218- 760378 147 970268.93 108.95 100.00 757736- 271879 147 476610.17 95.01 100.00 271523- 177233 147 212578.80 73.09 100.00 177042- 139581 147 159649.08 51.98 100.00 139530- 105963 147 119368.58 38.43 100.00 105502- 81728 147 93383.81 31.14 100.00 81663- 6099 147 49291.17 21.28 100.00 6064- 3341 147 4456.78 5.68 97.96 3337- 943 152 2500.76 4.31 71.71 ------------------------------------------------------------------------------------ 4714638- 943 1475 404786.21 55.55 96.88 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 147 747767.62 90.51 100.00 1.39- 1.09 147 814987.77 71.01 100.00 1.09- 0.96 147 379319.60 68.08 98.64 0.96- 0.85 147 420651.56 64.51 95.92 0.85- 0.80 147 491060.41 70.62 100.00 0.80- 0.73 147 277636.65 43.73 100.00 0.73- 0.70 147 234598.41 38.47 87.76 0.70- 0.65 147 332574.06 49.01 96.60 0.65- 0.62 147 186142.86 31.00 91.84 0.62- 0.58 152 171072.65 29.48 98.03 ------------------------------------------------------------------------------------ 4.82- 0.58 1475 404786.21 55.55 96.88 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:13:42 2018 Sorting 1475 observations 83 unique observations with > 7.00 F2/sig(F2) 1475 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 49 257 Total number of frames 257 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1475 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 12 66 Total number of frames 66 1186 observations > 7.00 F2/sig(F2) 1186 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 12 66 Total number of frames 66 Removing 'redundancy=1' reflections Average redundancy: 13.2 (Out of 1186 removed 2 = 1184, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1184 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 12 66 Total number of frames 66 90 unique data precomputed (should be 90) 90 unique data with 1184 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 13.2 (Out of 1184 removed 0 = 1184, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 1184 observations RMS deviation of equivalent data = 0.13169 Rint = 0.10442 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10423, wR= 0.13486 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06021, wR= 0.07812, Acormin=0.778, Acormax=1.282, Acor_av=1.004 F test: Probability=1.000, F= 2.983 Trying model 2 (ne=2, no=1)... Results: Rint= 0.06003, wR= 0.07605, Acormin=0.748, Acormax=1.298, Acor_av=0.979 F test: Probability=0.521, F= 1.003 Trying model 3 (ne=4, no=0)... Results: Rint= 0.04769, wR= 0.06200, Acormin=0.735, Acormax=1.331, Acor_av=0.960 F test: Probability=1.000, F= 1.581 Trying model 4 (ne=4, no=1)... Results: Rint= 0.04081, wR= 0.05464, Acormin=0.693, Acormax=1.333, Acor_av=0.932 F test: Probability=1.000, F= 1.362 Trying model 5 (ne=4, no=3)... Results: Rint= 0.03784, wR= 0.05054, Acormin=0.662, Acormax=1.335, Acor_av=0.929 F test: Probability=0.991, F= 1.156 Trying model 6 (ne=6, no=0)... Results: Rint= 0.04565, wR= 0.06001, Acormin=0.726, Acormax=1.324, Acor_av=0.955 F test: Probability=0.000, F= 0.685 Trying model 7 (ne=6, no=1)... Results: Rint= 0.03856, wR= 0.05264, Acormin=0.681, Acormax=1.326, Acor_av=0.929 F test: Probability=0.000, F= 0.958 Trying model 8 (ne=6, no=3)... Results: Rint= 0.03606, wR= 0.04804, Acormin=0.663, Acormax=1.349, Acor_av=0.947 F test: Probability=0.914, F= 1.088 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03154, wR= 0.04167, Acormin=0.623, Acormax=1.237, Acor_av=0.875 F test: Probability=1.000, F= 1.407 Trying model 10 (ne=8, no=0)... Results: Rint= 0.04185, wR= 0.05604, Acormin=0.704, Acormax=1.324, Acor_av=0.939 F test: Probability=0.000, F= 0.570 Trying model 11 (ne=8, no=1)... Results: Rint= 0.03343, wR= 0.04692, Acormin=0.663, Acormax=1.310, Acor_av=0.875 F test: Probability=0.000, F= 0.891 Trying model 12 (ne=8, no=3)... Results: Rint= 0.03168, wR= 0.04303, Acormin=0.587, Acormax=1.213, Acor_av=0.830 F test: Probability=0.000, F= 0.986 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02708, wR= 0.03741, Acormin=0.633, Acormax=1.218, Acor_av=0.858 F test: Probability=1.000, F= 1.334 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02577, wR= 0.03535, Acormin=0.632, Acormax=1.241, Acor_av=0.870 F test: Probability=0.912, F= 1.089 Final absorption model (ne=8, no=5): Rint= 0.02708, Acormin=0.633, Acormax=1.218, Acor_av=0.858 Combined refinement in use Rint: 0.10456 There are 66 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 5 (65 parameters) Refinement control: 130 pars with 8515 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13169 Using Levenberg-Marquardt: 0.00010 New wR= 0.03162 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10442 with corrections 0.02418 Rint for all data: 0.10456 with corrections 0.02442 3 observations identified as outliers and rejected Cycle 2 wR= 0.02995 Using Levenberg-Marquardt: 0.00001 New wR= 0.02819 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10380 with corrections 0.02115 Rint for all data: 0.10456 with corrections 0.02376 0 observations identified as outliers and rejected Cycle 3 wR= 0.02819 Using Levenberg-Marquardt: 0.00000 New wR= 0.02784 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10380 with corrections 0.02088 Rint for all data: 0.10456 with corrections 0.02355 0 observations identified as outliers and rejected Cycle 4 wR= 0.02784 Using Levenberg-Marquardt: 0.00000 New wR= 0.02766 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10380 with corrections 0.02073 Rint for all data: 0.10456 with corrections 0.02343 0 observations identified as outliers and rejected Cycle 5 wR= 0.02766 Using Levenberg-Marquardt: 0.00000 New wR= 0.02757 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10380 with corrections 0.02066 Rint for all data: 0.10456 with corrections 0.02336 0 observations identified as outliers and rejected Final wR= 0.02757 Final frame scales: Min= 0.8732 Max= 1.1299 Final absorption correction factors: Amin= 0.6989 Amax= 1.2597 PROFFIT INFO: Inet (after scale3 abspack): min=885.0961 max=5241219.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=110.3556 max=46450.1914 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1475 reflections read from tmp file 91 reflections are rejected (90 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 4 5 5 3 4 3 10 69 Initial Chi^2= 0.29296 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.92737 Current error model SIG(F2)^2 = 120.13*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 351.66*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 351.66*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5241220- 1257109 147 1968611.71 82.06 100.00 1232445- 739611 147 950089.64 38.01 100.00 736568- 286688 147 472380.46 37.70 100.00 286269- 178405 147 211849.16 25.73 100.00 178307- 143903 147 160632.36 18.68 100.00 143690- 103135 147 115852.22 13.18 100.00 102963- 82685 147 93739.77 11.25 100.00 82616- 5776 147 49441.56 7.96 87.76 5755- 3243 147 4323.28 2.85 15.65 3242- 885 152 2522.13 2.44 11.18 ------------------------------------------------------------------------------------ 5241220- 885 1475 401586.87 23.91 81.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 147 765181.01 55.00 95.92 1.39- 1.09 147 809078.10 42.31 87.07 1.09- 0.96 147 378194.50 25.20 82.31 0.96- 0.85 147 419333.86 23.26 84.35 0.85- 0.80 147 479994.42 24.90 87.76 0.80- 0.73 147 273583.98 15.68 71.43 0.73- 0.70 147 227680.53 13.86 73.47 0.70- 0.65 147 325526.22 17.37 89.12 0.65- 0.62 147 179160.63 11.26 72.11 0.62- 0.58 152 166143.69 10.74 69.08 ------------------------------------------------------------------------------------ 4.82- 0.58 1475 401586.87 23.91 81.22 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 147 765181.01 55.00 95.92 4.82- 1.09 294 787129.55 48.65 91.50 4.82- 0.96 441 650817.87 40.84 88.44 4.82- 0.85 588 592946.87 36.44 87.41 4.82- 0.80 735 570356.38 34.13 87.48 4.82- 0.73 882 520894.31 31.06 84.81 4.82- 0.70 1029 479006.63 28.60 83.19 4.82- 0.65 1176 459821.58 27.20 83.93 4.82- 0.62 1323 428637.03 25.43 82.62 4.82- 0.58 1475 401586.87 23.91 81.22 ------------------------------------------------------------------------------------ 4.82- 0.58 1475 401586.87 23.91 81.22 Scale applied to data: s=0.190795 (maximum obs:5241219.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.023; Rsigma 0.027: data 1475 -> merged 108 With outlier rejection... Rint 0.020; Rsigma 0.028: data 1467 -> merged 108 Rejected total: 8, method kkm 6, method Blessing 2 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585932, 4.831721 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 7.70 100.00 77 1.61 - 1.21 10 10 13.20 100.00 132 1.17 - 1.01 10 10 17.20 100.00 172 0.99 - 0.89 10 10 17.00 100.00 170 0.88 - 0.81 10 10 16.40 100.00 164 0.81 - 0.74 10 10 14.20 100.00 142 0.73 - 0.71 10 10 15.90 100.00 159 0.70 - 0.66 10 10 13.70 100.00 137 0.66 - 0.64 10 10 11.80 100.00 118 0.63 - 0.60 10 10 11.90 100.00 119 --------------------------------------------------------------- 5.92 - 0.60 100 100 13.90 100.00 1390 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:13:42 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917237 5.917084 5.916820 60.0719 90.0512 59.9763 1312 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.43 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 639 705 640 670 992 886 901 1312 N (int>3sigma) = 0 588 705 589 623 941 809 820 1196 Mean intensity = 0.0 52.4 26.6 52.4 59.9 43.3 63.3 60.5 61.2 Mean int/sigma = 0.0 27.2 24.4 27.3 28.4 26.2 29.0 28.4 28.4 Lattice type: P chosen Volume: 146.53 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Unitcell: 5.915 5.916 5.917 89.96 60.01 60.01 Niggli form: a.a = 34.988 b.b = 35.000 c.c = 35.012 b.c = 0.026 a.c = 17.493 a.b = 17.489 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.094 CUBIC F-lattice R(int) = 0.173 [ 1160] Vol = 586.1 Cell: 8.364 8.372 8.370 89.92 89.99 90.00 Volume: 586.11 Matrix: 1.0000 0.0000 1.0000 1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.034 RHOMBOHEDRAL R-lattice R(int) = 0.167 [ 893] Vol = 439.6 Cell: 5.915 5.916 14.503 90.07 90.00 119.99 Volume: 439.59 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.034 RHOMBOHEDRAL R-lattice R(int) = 0.163 [ 262] Vol = 439.6 Trigonal Cell: 5.915 5.916 14.503 90.07 90.00 119.99 Volume: 439.59 Matrix:-1.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.060 TETRAGONAL I-lattice R(int) = 0.154 [ 932] Vol = 293.1 Cell: 5.917 5.917 8.370 89.95 89.94 89.95 Volume: 293.06 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.060 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 933] Vol = 293.1 Cell: 5.917 5.917 8.370 89.94 89.95 89.95 Volume: 293.06 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.013 ORTHORHOMBIC I-lattice R(int) = 0.136 [ 880] Vol = 293.1 Cell: 5.915 8.364 5.923 89.99 89.99 90.00 Volume: 293.06 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.057 MONOCLINIC I-lattice R(int) = 0.134 [ 717] Vol = 293.1 Cell: 5.917 5.917 8.370 90.05 90.06 89.95 Volume: 293.06 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.013 MONOCLINIC I-lattice R(int) = 0.122 [ 618] Vol = 293.1 Cell: 5.915 8.364 5.923 90.01 90.01 90.00 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.005 MONOCLINIC I-lattice R(int) = 0.128 [ 598] Vol = 293.1 Cell: 8.364 5.915 5.923 90.01 90.01 90.00 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.100 [ 356] Vol = 146.5 Cell: 5.915 5.916 5.917 89.96 60.01 60.01 Volume: 146.53 Matrix: 1.0000 -1.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 705 0 882 894 1312 N (int>3sigma) = 0 0 0 0 705 0 807 815 1196 Mean intensity = 0.0 0.0 0.0 0.0 26.6 0.0 62.1 61.8 61.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 28.5 28.2 28.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.068 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 16 16 99 288 N I>3s 16 16 73 288 0.9 0.9 0.7 31.3 6.9 6.9 4.1 29.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.173 1081 Fd-3m 1 1 227 C N N N N 37 2284 0.176 1118 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364202 8.371680 8.370381 89.9193 89.9900 89.9960 ZERR 1.00 0.000355 0.002080 0.004573 0.0026 0.0151 0.0019 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4474999- 616787 329 324 27 12.0 1349221.53 55.31 0.017 0.019 597922- 123496 449 447 27 16.6 233921.05 25.94 0.024 0.028 120008- 11487 368 368 27 13.6 87740.16 10.81 0.037 0.045 8860- 2135 329 328 27 12.1 3700.95 2.70 0.152 0.184 ------------------------------------------------------------------------------------------- 4474999- 2135 1475 1467 108 13.6 392101.42 23.44 0.020 0.022 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 359 352 27 13.0 667541.67 42.96 0.018 0.019 0.016 1.01-0.78 447 446 28 15.9 383615.81 21.48 0.015 0.019 0.028 0.76-0.65 403 403 28 14.4 292061.58 16.05 0.023 0.027 0.039 0.65-0.59 266 266 25 10.6 193400.90 12.07 0.034 0.037 0.055 ------------------------------------------------------------------------------------------------------ inf-0.59 1475 1467 108 13.6 392101.42 23.44 0.020 0.022 0.028 inf-0.60 1396 1388 99 14.0 407142.99 24.23 0.019 0.022 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 352 27 27 100.0 13.0 667541.67 162.37 0.018 0.005 1.01-0.78 446 28 28 100.0 15.9 383615.81 90.59 0.015 0.007 0.76-0.65 403 28 28 100.0 14.4 292061.58 64.87 0.023 0.012 0.65-0.59 266 26 25 96.2 10.6 193400.90 44.35 0.034 0.020 -------------------------------------------------------------------------------------------- inf-0.59 1467 109 108 99.1 13.6 392101.42 92.36 0.020 0.008 inf-0.60 1388 99 99 100.0 14.0 407142.99 95.74 0.019 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:20:40 2018) ID: 2932; threads 39; handles 878; mem 518432.00 (1237700.00)kB; time: 1w 4d 23h 26m 10s MEMORY INFO: Memory PF:0.0, Ph:217.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.3,peak PF: 697.1, WS: 297.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:217.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.1,peak PF: 697.1, WS: 299.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:20:40 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000019 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000015 0.000012 0.000011 ) 5.91502 ( 0.00096 ) 5.91640 ( 0.00096 ) 5.92265 ( 0.00076 ) 60.05206 ( 0.01525 ) 89.98756 ( 0.01179 ) 60.01743 ( 0.01699 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:20:40 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000019 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000015 0.000012 0.000011 ) M - matrix: 0.021572 -0.014384 0.007196 ( 0.000005 0.000003 0.000003 ) -0.014384 0.028723 -0.014344 ( 0.000003 0.000004 0.000003 ) 0.007196 -0.014344 0.021534 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9150(10) 5.9164(10) 5.9227(8) 60.052(15) 89.988(12) 60.017(17) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.083 ( 0.108) | 1.073 ( 0.135) | 1.145 ( 0.399) | 0.84- 0.81 | 44 | 1.105 ( 0.099) | 1.023 ( 0.124) | 1.367 ( 0.511) | 0.81- 0.73 | 44 | 1.098 ( 0.089) | 0.991 ( 0.126) | 1.342 ( 0.507) | 0.73- 0.69 | 44 | 1.087 ( 0.077) | 0.931 ( 0.109) | 1.374 ( 0.487) | 0.69- 0.66 | 44 | 1.078 ( 0.073) | 0.883 ( 0.089) | 1.403 ( 0.484) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.062 ( 0.110) | 0.998 ( 0.252) | 1.318 ( 0.893) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070034 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068375 -0.065763 -0.010701 ( 0.000027 0.000027 0.000015 ) 0.109065 -0.152749 0.115659 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028586 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9266(15) 5.9308(15) 5.9443(11) 60.01(2) 90.018(18) 60.02(3) V = 147.79(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070138 0.030665 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109140 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9312(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070138 0.030665 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109140 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9312(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.708) | 1.567 ( 2.300) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.170 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.142) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.029 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.993 ( 0.128) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.383 ( 0.483) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.269 ( 0.497) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.063 ( 0.108) | 1.003 ( 0.281) | 1.322 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb PROFFITPEAK info: 953 peaks in the peak location table UB fit with 416 obs out of 443 (total:443,skipped:0) (93.91%) UB - matrix: -0.069936 0.031071 0.088948 ( 0.000070 0.000061 0.000100 ) -0.068962 -0.065568 -0.010320 ( 0.000054 0.000047 0.000077 ) 0.109079 -0.152856 0.116048 ( 0.000072 0.000063 0.000103 ) M - matrix: 0.021545 -0.014325 0.007149 ( 0.000020 0.000015 0.000018 ) -0.014325 0.028630 -0.014298 ( 0.000015 0.000021 0.000019 ) 0.007149 -0.014298 0.021485 ( 0.000018 0.000019 0.000030 ) unit cell: 5.915(4) 5.923(3) 5.922(4) 60.03(7) 89.98(5) 60.01(6) V = 146.86(15) UB fit with 416 obs out of 443 (total:443,skipped:0) (93.91%) UB - matrix: -0.069936 0.031071 0.088948 ( 0.000070 0.000061 0.000100 ) -0.068962 -0.065568 -0.010320 ( 0.000054 0.000047 0.000077 ) 0.109079 -0.152856 0.116048 ( 0.000072 0.000063 0.000103 ) M - matrix: 0.021545 -0.014325 0.007149 ( 0.000020 0.000015 0.000018 ) -0.014325 0.028630 -0.014298 ( 0.000015 0.000021 0.000019 ) 0.007149 -0.014298 0.021485 ( 0.000018 0.000019 0.000030 ) unit cell: 5.915(4) 5.923(3) 5.922(4) 60.03(7) 89.98(5) 60.01(6) V = 146.86(15) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB fit with 417 obs out of 443 (total:443,skipped:0) (94.13%) UB - matrix: -0.069930 0.031073 0.088962 ( 0.000070 0.000061 0.000099 ) -0.068960 -0.065566 -0.010315 ( 0.000054 0.000047 0.000076 ) 0.109098 -0.152846 0.116056 ( 0.000073 0.000064 0.000104 ) M - matrix: 0.021548 -0.014327 0.007152 ( 0.000020 0.000015 0.000018 ) -0.014327 0.028626 -0.014298 ( 0.000015 0.000021 0.000019 ) 0.007152 -0.014298 0.021490 ( 0.000018 0.000019 0.000030 ) unit cell: 5.915(4) 5.924(3) 5.922(4) 60.04(7) 89.98(5) 60.01(6) V = 146.85(15) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Run 3 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 594 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069929 0.031073 0.088963 ( 0.000070 0.000061 0.000099 ) -0.068959 -0.065566 -0.010315 ( 0.000054 0.000047 0.000076 ) 0.109099 -0.152846 0.116057 ( 0.000073 0.000064 0.000104 ) M - matrix: 0.021548 -0.014327 0.007152 ( 0.000020 0.000015 0.000018 ) -0.014327 0.028626 -0.014298 ( 0.000015 0.000021 0.000019 ) 0.007152 -0.014298 0.021490 ( 0.000018 0.000019 0.000030 ) UB fit with 417 obs out of 443 (total:443,skipped:0) (94.13%) unit cell: 5.915(4) 5.924(3) 5.921(4) 60.04(7) 89.98(5) 60.01(6) V = 146.84(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 417 obs out of 443 (total:443,skipped:0) (94.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb 5 of 333 peaks identified as outliers and rejected 328 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 328 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 328 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.47 | 33 | 1.017 ( 0.250) | 1.103 ( 0.423) | 1.013 ( 0.349) | 1.47- 1.15 | 33 | 1.058 ( 0.125) | 1.192 ( 0.535) | 0.968 ( 0.252) | 1.12- 0.98 | 33 | 1.017 ( 0.088) | 1.021 ( 0.092) | 1.051 ( 0.507) | 0.96- 0.89 | 33 | 1.006 ( 0.098) | 1.010 ( 0.108) | 1.021 ( 0.402) | 0.89- 0.82 | 33 | 1.020 ( 0.069) | 0.981 ( 0.113) | 1.174 ( 0.418) | 0.81- 0.73 | 33 | 0.995 ( 0.085) | 0.940 ( 0.104) | 1.060 ( 0.457) | 0.73- 0.70 | 33 | 0.983 ( 0.042) | 0.904 ( 0.056) | 1.370 ( 0.543) | 0.70- 0.65 | 33 | 0.952 ( 0.052) | 0.849 ( 0.054) | 1.206 ( 0.431) | 0.65- 0.62 | 33 | 0.930 ( 0.049) | 0.831 ( 0.032) | 1.254 ( 0.463) | 0.62- 0.59 | 31 | 0.911 ( 0.044) | 0.813 ( 0.039) | 1.259 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 328 | 0.989 ( 0.116) | 0.965 ( 0.256) | 1.137 ( 0.457) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) UB - matrix: -0.069991 0.030994 0.089140 ( 0.000036 0.000030 0.000048 ) -0.068598 -0.065932 -0.010147 ( 0.000019 0.000016 0.000025 ) 0.109071 -0.153038 0.116289 ( 0.000028 0.000023 0.000037 ) M - matrix: 0.021501 -0.014338 0.007141 ( 0.000008 0.000006 0.000007 ) -0.014338 0.028728 -0.014365 ( 0.000006 0.000008 0.000007 ) 0.007141 -0.014365 0.021572 ( 0.000007 0.000007 0.000012 ) unit cell: 5.9223(14) 5.9183(13) 5.913(2) 59.96(3) 89.89(2) 59.97(2) V = 146.55(7) OTKP changes: 328 1 1 1 OTKP changes: 328 1 1 1 OTKP changes: 328 1 1 1 UB - matrix: -0.069890 0.031037 0.088899 ( 0.000033 0.000028 0.000044 ) -0.068721 -0.065755 -0.010194 ( 0.000017 0.000014 0.000023 ) 0.108975 -0.152796 0.116245 ( 0.000026 0.000021 0.000034 ) M - matrix: 0.021483 -0.014301 0.007155 ( 0.000008 0.000005 0.000007 ) -0.014301 0.028634 -0.014332 ( 0.000005 0.000007 0.000007 ) 0.007155 -0.014332 0.021520 ( 0.000007 0.000007 0.000011 ) UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) unit cell: 5.9232(13) 5.9256(12) 5.9220(18) 59.98(3) 89.99(2) 60.04(2) V = 147.03(6) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 592 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069890 0.031037 0.088899 ( 0.000033 0.000028 0.000044 ) -0.068721 -0.065755 -0.010194 ( 0.000017 0.000014 0.000023 ) 0.108975 -0.152796 0.116245 ( 0.000026 0.000021 0.000034 ) M - matrix: 0.021483 -0.014301 0.007155 ( 0.000008 0.000005 0.000007 ) -0.014301 0.028634 -0.014332 ( 0.000005 0.000007 0.000007 ) 0.007155 -0.014332 0.021520 ( 0.000007 0.000007 0.000011 ) UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) unit cell: 5.9232(13) 5.9256(12) 5.9220(18) 59.98(3) 89.99(2) 60.04(2) V = 147.03(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb 6 of 336 peaks identified as outliers and rejected 330 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 330 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 330 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 33 | 1.018 ( 0.254) | 1.092 ( 0.356) | 1.015 ( 0.344) | 1.42- 1.17 | 33 | 1.044 ( 0.140) | 1.162 ( 0.527) | 1.052 ( 0.525) | 1.15- 0.99 | 33 | 1.006 ( 0.092) | 1.056 ( 0.250) | 1.072 ( 0.513) | 0.99- 0.89 | 33 | 1.017 ( 0.088) | 1.029 ( 0.113) | 0.985 ( 0.342) | 0.89- 0.82 | 33 | 1.020 ( 0.070) | 0.977 ( 0.105) | 1.156 ( 0.422) | 0.82- 0.74 | 33 | 0.994 ( 0.087) | 0.938 ( 0.106) | 1.093 ( 0.464) | 0.73- 0.70 | 33 | 0.984 ( 0.042) | 0.905 ( 0.057) | 1.337 ( 0.544) | 0.70- 0.66 | 33 | 0.953 ( 0.053) | 0.851 ( 0.053) | 1.213 ( 0.446) | 0.66- 0.62 | 33 | 0.931 ( 0.049) | 0.832 ( 0.035) | 1.264 ( 0.468) | 0.62- 0.59 | 33 | 0.914 ( 0.043) | 0.810 ( 0.033) | 1.285 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 330 | 0.988 ( 0.117) | 0.965 ( 0.252) | 1.147 ( 0.478) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 118 | 1.128 ( 0.136) | 1.270 ( 0.492) | 1.271 ( 1.453) | 13.4-19.4 | 118 | 1.084 ( 0.060) | 1.134 ( 0.258) | 1.214 ( 0.528) | 19.4-23.4 | 118 | 1.071 ( 0.071) | 1.110 ( 0.240) | 1.153 ( 0.478) | 23.4-27.5 | 118 | 1.038 ( 0.089) | 1.088 ( 0.333) | 1.227 ( 0.573) | 27.5-31.0 | 118 | 1.019 ( 0.086) | 1.005 ( 0.194) | 1.256 ( 0.510) | 31.1-34.1 | 118 | 0.988 ( 0.090) | 0.923 ( 0.105) | 1.214 ( 0.520) | 34.3-37.0 | 118 | 0.968 ( 0.082) | 0.892 ( 0.095) | 1.237 ( 0.503) | 37.0-39.9 | 118 | 0.954 ( 0.102) | 0.886 ( 0.167) | 1.168 ( 0.546) | 39.9-42.9 | 119 | 0.933 ( 0.090) | 0.842 ( 0.091) | 1.181 ( 0.502) | 42.9-49.9 | 114 | 0.943 ( 0.087) | 0.818 ( 0.064) | 1.177 ( 0.458) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1177 | 1.013 ( 0.111) | 0.997 ( 0.278) | 1.210 ( 0.671) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0100 b=1.27 e3 dimension: a=0.0027 b=0.98 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706998 Maximum peak integral for reflections I/sig<= 10000 - raw: 23928508 lp-corr: 2429818 PROFFITPEAK - Finished at Tue Mar 27 14:20:57 2018 PROFFITMAIN - Started at Tue Mar 27 14:20:57 2018 OTKP changes: 1177 2 3 3 OTKP changes: 1177 2 3 3 UB - matrix: -0.070251 0.031084 0.088886 ( 0.000017 0.000014 0.000014 ) -0.068716 -0.065811 -0.010602 ( 0.000018 0.000014 0.000014 ) 0.109216 -0.153094 0.116344 ( 0.000014 0.000011 0.000011 ) M - matrix: 0.021585 -0.014382 0.007191 ( 0.000005 0.000003 0.000003 ) -0.014382 0.028735 -0.014351 ( 0.000003 0.000004 0.000003 ) 0.007191 -0.014351 0.021549 ( 0.000003 0.000003 0.000004 ) UB fit with 1177 obs out of 1177 (total:1177,skipped:0) (100.00%) unit cell: 5.9134(9) 5.9147(9) 5.9145(7) 60.058(14) 90.033(11) 59.993(16) V = 146.35(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070074 0.030681 0.088931 ( 0.000028 0.000028 0.000016 ) -0.068222 -0.066129 -0.010548 ( 0.000025 0.000024 0.000014 ) 0.109090 -0.153074 0.116013 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021465 -0.014337 0.007144 ( 0.000007 0.000006 0.000004 ) -0.014337 0.028746 -0.014333 ( 0.000006 0.000008 0.000004 ) 0.007144 -0.014333 0.021479 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9285(14) 5.9141(14) 5.9247(11) 60.02(2) 89.981(17) 59.99(2) V = 146.94(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070313 0.030920 0.088795 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066112 -0.010697 ( 0.000024 0.000023 0.000013 ) 0.109317 -0.153269 0.116349 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021573 -0.014407 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014407 0.028818 -0.014380 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014380 0.021536 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9167(13) 5.9082(13) 5.9189(10) 60.05(2) 90.074(16) 60.00(2) V = 146.32(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.806) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070313 0.030920 0.088795 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066112 -0.010697 ( 0.000024 0.000023 0.000013 ) 0.109317 -0.153269 0.116349 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021573 -0.014407 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014407 0.028818 -0.014380 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014380 0.021536 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9167(13) 5.9082(13) 5.9189(10) 60.05(2) 90.074(16) 60.00(2) V = 146.32(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070313 0.030920 0.088795 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066112 -0.010697 ( 0.000024 0.000023 0.000013 ) 0.109317 -0.153269 0.116349 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021573 -0.014407 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014407 0.028818 -0.014380 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014380 0.021536 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9167(13) 5.9082(13) 5.9189(10) 60.05(2) 90.074(16) 60.00(2) V = 146.32(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070407 0.031323 0.088619 ( 0.000025 0.000022 0.000027 ) -0.068591 -0.065973 -0.010271 ( 0.000031 0.000027 0.000033 ) 0.109003 -0.152702 0.116261 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021543 -0.014325 0.007138 ( 0.000007 0.000005 0.000005 ) -0.014325 0.028651 -0.014300 ( 0.000005 0.000006 0.000005 ) 0.007138 -0.014300 0.021475 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(16) 5.9211(16) 5.9235(13) 60.02(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070351 0.031190 0.088834 ( 0.000023 0.000020 0.000025 ) -0.068766 -0.065861 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109155 -0.153132 0.116560 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021593 -0.014380 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014380 0.028760 -0.014397 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014397 0.021585 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9103(16) 5.9172(16) 5.9155(12) 59.94(2) 89.945(19) 60.01(3) V = 146.23(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.806) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070351 0.031190 0.088834 ( 0.000023 0.000020 0.000025 ) -0.068766 -0.065861 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109155 -0.153132 0.116560 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021593 -0.014380 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014380 0.028760 -0.014397 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014397 0.021585 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9103(16) 5.9172(16) 5.9155(12) 59.94(2) 89.945(19) 60.01(3) V = 146.23(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070351 0.031190 0.088834 ( 0.000023 0.000020 0.000025 ) -0.068766 -0.065861 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109155 -0.153132 0.116560 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021593 -0.014380 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014380 0.028760 -0.014397 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014397 0.021585 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9103(16) 5.9172(16) 5.9155(12) 59.94(2) 89.945(19) 60.01(3) V = 146.23(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) UB - matrix: -0.070027 0.031034 0.088966 ( 0.000034 0.000028 0.000045 ) -0.068592 -0.065970 -0.010176 ( 0.000021 0.000017 0.000027 ) 0.108950 -0.152837 0.116256 ( 0.000027 0.000022 0.000035 ) M - matrix: 0.021479 -0.014300 0.007134 ( 0.000008 0.000006 0.000007 ) -0.014300 0.028674 -0.014336 ( 0.000006 0.000007 0.000007 ) 0.007134 -0.014336 0.021534 ( 0.000007 0.000007 0.000011 ) unit cell: 5.9216(14) 5.9193(13) 5.9177(19) 59.98(3) 89.94(2) 60.04(2) V = 146.78(6) OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 UB - matrix: -0.070024 0.030908 0.089156 ( 0.000034 0.000028 0.000044 ) -0.068874 -0.065837 -0.010318 ( 0.000017 0.000014 0.000023 ) 0.109271 -0.153161 0.116388 ( 0.000026 0.000022 0.000034 ) M - matrix: 0.021587 -0.014366 0.007185 ( 0.000008 0.000005 0.000007 ) -0.014366 0.028748 -0.014391 ( 0.000005 0.000007 0.000007 ) 0.007185 -0.014391 0.021601 ( 0.000007 0.000007 0.000011 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9091(13) 5.9147(12) 5.9114(18) 59.97(3) 89.98(2) 60.04(2) V = 146.13(6) Run 3 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.806) HKL list info: 583 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070024 0.030908 0.089156 ( 0.000034 0.000028 0.000044 ) -0.068874 -0.065837 -0.010318 ( 0.000017 0.000014 0.000023 ) 0.109271 -0.153161 0.116388 ( 0.000026 0.000022 0.000034 ) M - matrix: 0.021587 -0.014366 0.007185 ( 0.000008 0.000005 0.000007 ) -0.014366 0.028748 -0.014391 ( 0.000005 0.000007 0.000007 ) 0.007185 -0.014391 0.021601 ( 0.000007 0.000007 0.000011 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9091(13) 5.9147(12) 5.9114(18) 59.97(3) 89.98(2) 60.04(2) V = 146.13(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.070024 0.030908 0.089156 ( 0.000034 0.000028 0.000044 ) -0.068874 -0.065837 -0.010318 ( 0.000017 0.000014 0.000023 ) 0.109271 -0.153161 0.116388 ( 0.000026 0.000022 0.000034 ) M - matrix: 0.021587 -0.014366 0.007185 ( 0.000008 0.000005 0.000007 ) -0.014366 0.028748 -0.014391 ( 0.000005 0.000007 0.000007 ) 0.007185 -0.014391 0.021601 ( 0.000007 0.000007 0.000011 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9091(13) 5.9147(12) 5.9114(18) 59.97(3) 89.98(2) 60.04(2) V = 146.13(6) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070253 0.031080 0.088843 ( 0.000017 0.000014 0.000014 ) -0.068713 -0.065752 -0.010666 ( 0.000018 0.000014 0.000014 ) 0.109237 -0.153124 0.116376 ( 0.000014 0.000011 0.000011 ) M - matrix: 0.021590 -0.014392 0.007204 ( 0.000005 0.000003 0.000003 ) -0.014392 0.028736 -0.014357 ( 0.000003 0.000004 0.000003 ) 0.007204 -0.014357 0.021550 ( 0.000003 0.000003 0.000004 ) UB fit with 1177 obs out of 1177 (total:1177,skipped:0) (100.00%) unit cell: 5.9147(9) 5.9163(9) 5.9156(7) 60.059(15) 90.052(11) 59.984(16) V = 146.40(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 58 reflections under beam stop or inside a detector rejection region 9 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof 1621 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:21:01 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.806) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.806) Run 3 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.806) PROFFIT INFO: signal sum: min=237.0000 max=20592796.0000 PROFFIT INFO: signal sum lp corr: min=585.8264 max=2947611.5937 PROFFIT INFO: background sum: min=1049.0000 max=26505.0000 PROFFIT INFO: background sum sig2: min=524.0000 max=12084.0000 PROFFIT INFO: num of signal pixels: min=51 max=520 PROFFIT INFO: Inet: min=937.3222 max=4716178.5000 PROFFIT INFO: sig(Inet): min=96.4556 max=47442.6602 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=229.72 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 8 51 147 326 360 617 1056 1470 1621 Percent 0.0 0.0 0.5 3.1 9.1 20.1 22.2 38.1 65.1 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1621 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1621 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4716179- 1238071 162 1951891.10 125.78 100.00 1237685- 752787 162 957148.92 109.30 100.00 746269- 272705 162 481742.42 94.70 100.00 272160- 178378 162 213961.03 74.16 100.00 178076- 136588 162 158330.74 51.75 100.00 136516- 104448 162 117976.05 38.11 100.00 104317- 81451 162 92634.23 30.93 100.00 81125- 6119 162 49271.52 21.44 100.00 6112- 3334 162 4467.97 5.61 98.15 3331- 937 163 2480.16 4.28 70.55 ------------------------------------------------------------------------------------ 4716179- 937 1621 402743.34 55.57 96.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 162 746212.68 87.06 98.77 1.41- 1.07 162 592025.33 71.22 98.15 1.07- 0.96 162 418598.98 63.73 97.53 0.96- 0.82 162 423621.77 53.73 96.30 0.82- 0.74 162 419807.41 57.82 96.30 0.74- 0.67 162 372595.78 53.53 97.53 0.67- 0.62 162 290255.45 47.97 98.15 0.62- 0.57 162 323144.54 48.05 93.21 0.57- 0.52 162 233670.23 38.52 96.30 0.52- 0.40 163 208699.03 34.24 96.32 ------------------------------------------------------------------------------------ 5.26- 0.40 1621 402743.34 55.57 96.85 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:21:01 2018 Sorting 1621 observations 231 unique observations with > 7.00 F2/sig(F2) 1621 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 74 282 Total number of frames 282 Maximum number of 231 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1621 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 37 143 Total number of frames 143 1310 observations > 7.00 F2/sig(F2) 1310 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 37 143 Total number of frames 143 Removing 'redundancy=1' reflections Average redundancy: 5.6 (Out of 1310 removed 53 = 1257, unique = 224) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1257 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 37 143 Total number of frames 143 224 unique data precomputed (should be 224) 224 unique data with 1257 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 5.6 (Out of 1257 removed 0 = 1257, unique = 224) 224 unique data precomputed (should be 224) 224 unique data with 1257 observations RMS deviation of equivalent data = 0.69804 Rint = 0.66390 5 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.64998, wR= 4.10884 Trying model 1 (ne=2, no=0)... Results: Rint= 0.72023, wR= 3.00016, Acormin=-0.033, Acormax=2.136, Acor_av=0.624 F test: Probability=0.000, F= 0.810 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88971, wR= 3.17155, Acormin=-0.369, Acormax=1.863, Acor_av=0.346 F test: Probability=0.000, F= 0.530 Trying model 3 (ne=4, no=0)... Results: Rint= 0.74662, wR= 2.49416, Acormin=-0.145, Acormax=2.199, Acor_av=0.495 F test: Probability=0.000, F= 0.748 Trying model 4 (ne=4, no=1)... Results: Rint= 0.87861, wR= 2.70934, Acormin=-0.505, Acormax=2.029, Acor_av=0.292 F test: Probability=0.000, F= 0.538 Trying model 5 (ne=4, no=3)... Results: Rint= 0.95701, wR= 2.13199, Acormin=-1.122, Acormax=1.451, Acor_av=0.088 F test: Probability=0.000, F= 0.451 Trying model 6 (ne=6, no=0)... Results: Rint= 0.81253, wR= 2.58661, Acormin=-0.267, Acormax=2.723, Acor_av=0.404 F test: Probability=0.000, F= 0.623 Trying model 7 (ne=6, no=1)... Results: Rint= 0.94159, wR= 2.93413, Acormin=-0.630, Acormax=2.229, Acor_av=0.197 F test: Probability=0.000, F= 0.463 Trying model 8 (ne=6, no=3)... Results: Rint= 0.97240, wR= 2.68458, Acormin=-1.147, Acormax=1.498, Acor_av=0.065 F test: Probability=0.000, F= 0.431 Trying model 9 (ne=6, no=5)... Results: Rint= 0.99553, wR= 2.23911, Acormin=-0.496, Acormax=1.861, Acor_av=0.012 F test: Probability=0.000, F= 0.406 Trying model 10 (ne=8, no=0)... Results: Rint= 0.88009, wR= 2.13817, Acormin=-0.712, Acormax=3.198, Acor_av=0.297 F test: Probability=0.000, F= 0.522 Trying model 11 (ne=8, no=1)... Results: Rint= 1.02068, wR= 2.15958, Acormin=-1.024, Acormax=1.355, Acor_av=0.030 F test: Probability=0.000, F= 0.387 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97372, wR= 1.56997, Acormin=-0.038, Acormax=0.076, Acor_av=0.002 F test: Probability=0.000, F= 0.422 Trying model 13 (ne=8, no=5)... Results: Rint= 0.97182, wR= 1.66861, Acormin=-0.037, Acormax=0.076, Acor_av=0.003 F test: Probability=0.000, F= 0.419 Trying model 14 (ne=8, no=7)... Results: Rint= 0.98912, wR= 1.46985, Acormin=-0.046, Acormax=0.069, Acor_av=0.001 F test: Probability=0.000, F= 0.398 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.83114 There are 143 active scales (one needs to be fixed) Refinement control: frame scale #137 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 147 pars with 10878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.69804 Using Levenberg-Marquardt: 0.00010 New wR= 0.68045 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66390 with corrections 0.64532 Rint for all data: 0.83114 with corrections 0.81550 5 observations identified as outliers and rejected Cycle 2 wR= 0.65336 Using Levenberg-Marquardt: 0.00001 New wR= 0.65185 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64998 with corrections 0.63154 Rint for all data: 0.83114 with corrections 0.81609 7 observations identified as outliers and rejected Cycle 3 wR= 0.62941 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62302 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63636 with corrections 0.62152 Rint for all data: 0.83114 with corrections 0.81838 4 observations identified as outliers and rejected Cycle 4 wR= 0.61677 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.68964 Using Levenberg-Marquardt: 0.10000 New wR= 0.61582 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63355 with corrections 0.62101 Rint for all data: 0.83114 with corrections 0.82015 4 observations identified as outliers and rejected Cycle 5 wR= 0.60472 Using Levenberg-Marquardt: 0.01000 New wR= 0.60951 Using Levenberg-Marquardt: 0.10000 New wR= 0.60362 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63050 with corrections 0.62263 Rint for all data: 0.83114 with corrections 0.82274 2 observations identified as outliers and rejected Final wR= 0.60362 Final frame scales: Min= 0.6421 Max= 2.9977 Final absorption correction factors: Amin= 0.3623 Amax= 1.7778 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=673.9944 max=6584126.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=118.1234 max=68897.5313 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/108 1620 reflections read from tmp file 1263 reflections are rejected (1156 as outliers, 107 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 73 39 15 3 2 1 Initial Chi^2= 0.84485 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.98474 Current error model SIG(F2)^2 = 378.87*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 373.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 373.09*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6584126- 1234841 162 2096125.94 76.88 100.00 1231734- 600685 162 886633.75 39.88 100.00 600259- 293169 162 423641.12 34.68 100.00 292499- 186794 162 233183.06 25.55 100.00 186738- 131847 162 156902.41 17.12 100.00 131844- 97462 162 114399.92 13.95 100.00 97199- 62692 162 78619.22 11.30 100.00 62407- 6179 162 36863.62 8.40 87.65 6179- 3015 162 4133.97 2.71 16.67 3008- 674 162 2227.92 2.27 7.41 ------------------------------------------------------------------------------------ 6584126- 674 1620 403273.09 23.27 81.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 162 942366.05 51.46 94.44 1.41- 1.07 162 639899.46 35.26 88.27 1.07- 0.96 162 468988.20 24.69 84.57 0.93- 0.82 162 430655.70 21.92 77.16 0.82- 0.74 162 410669.59 22.11 82.72 0.74- 0.67 162 335374.84 18.67 76.54 0.67- 0.62 162 246299.56 16.71 80.25 0.62- 0.57 162 263710.58 16.51 79.01 0.57- 0.52 162 168041.79 13.44 76.54 0.52- 0.40 162 126725.15 11.98 72.22 ------------------------------------------------------------------------------------ 5.26- 0.40 1620 403273.09 23.27 81.17 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 162 942366.05 51.46 94.44 5.26- 1.07 324 791132.76 43.36 91.36 5.26- 0.96 486 683751.24 37.13 89.09 5.26- 0.82 648 620477.35 33.33 86.11 5.26- 0.74 810 578515.80 31.09 85.43 5.26- 0.67 972 537992.31 29.02 83.95 5.26- 0.62 1134 496321.91 27.26 83.42 5.26- 0.57 1296 467245.50 25.92 82.87 5.26- 0.52 1458 434000.64 24.53 82.17 5.26- 0.40 1620 403273.09 23.27 81.17 ------------------------------------------------------------------------------------ 5.26- 0.40 1620 403273.09 23.27 81.17 Scale applied to data: s=0.151880 (maximum obs:6584126.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.822; Rsigma 0.027: data 1620 -> merged 300 With outlier rejection... Rint 0.694; Rsigma 0.029: data 1464 -> merged 300 Rejected total: 156, method kkm 145, method Blessing 11 Completeness direct cell (a, b, c) = (5.270, 5.270, 5.270), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404225, 5.270444 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 7.80 100.00 117 1.46 - 1.12 15 15 11.33 100.00 170 1.08 - 0.96 15 15 9.80 100.00 147 0.96 - 0.85 15 15 8.80 100.00 132 0.85 - 0.79 15 15 7.60 100.00 114 0.79 - 0.73 15 15 7.00 100.00 105 0.73 - 0.69 15 15 5.87 100.00 88 0.69 - 0.65 15 15 6.13 100.00 92 0.65 - 0.63 15 15 3.93 100.00 59 0.63 - 0.60 21 21 4.24 100.00 89 --------------------------------------------------------------- 5.91 - 0.60 156 156 7.13 100.00 1113 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:21:01 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914653 5.916290 5.915567 60.0592 90.0524 59.9835 1464 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 722 784 722 734 1114 988 1000 1464 N (int>3sigma) = 0 569 784 569 576 961 799 811 1185 Mean intensity = 0.0 48.3 24.4 48.2 55.1 39.9 57.2 54.7 55.9 Mean int/sigma = 0.0 20.9 18.7 20.9 22.1 20.1 23.1 22.6 22.5 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.914 5.914 5.915 60.02 60.08 60.02 Niggli form: a.a = 34.970 b.b = 34.975 c.c = 34.983 b.c = 17.478 a.c = 17.446 a.b = 17.476 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.224 [ 1311] Vol = 585.6 Cell: 8.361 8.368 8.369 90.07 90.01 90.03 Volume: 585.60 Matrix: 1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.031 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 1060] Vol = 439.2 Cell: 5.916 5.921 14.482 90.01 89.97 120.02 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.031 RHOMBOHEDRAL R-lattice R(int) = 0.171 [ 327] Vol = 439.2 Trigonal Cell: 5.916 5.921 14.482 90.01 89.97 120.02 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.041 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 1041] Vol = 439.2 Cell: 5.914 5.916 14.498 89.94 90.07 120.01 Volume: 439.20 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.041 RHOMBOHEDRAL R-lattice R(int) = 0.202 [ 310] Vol = 439.2 Trigonal Cell: 5.914 5.916 14.498 89.94 90.07 120.01 Volume: 439.20 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.168 [ 1054] Vol = 292.8 Cell: 5.914 5.916 8.369 89.96 89.94 89.95 Volume: 292.80 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.146 ORTHORHOMBIC I-lattice R(int) = 0.196 [ 1082] Vol = 292.8 Cell: 5.915 8.368 5.916 90.03 89.95 90.07 Volume: 292.80 Matrix: 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.031 MONOCLINIC I-lattice R(int) = 0.168 [ 854] Vol = 292.8 Cell: 5.915 5.916 8.368 89.97 90.07 90.05 Volume: 292.80 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.033 MONOCLINIC I-lattice R(int) = 0.158 [ 814] Vol = 292.8 Cell: 5.914 5.916 8.369 90.04 90.06 89.95 Volume: 292.80 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.152 [ 775] Vol = 292.8 Cell: 5.916 5.914 8.369 90.06 90.04 89.95 Volume: 292.80 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.052 MONOCLINIC I-lattice R(int) = 0.152 [ 775] Vol = 292.8 Cell: 8.369 5.914 5.916 89.95 90.04 90.06 Volume: 292.80 Matrix: 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.114 [ 474] Vol = 146.4 Cell: 5.914 5.914 5.915 60.02 60.08 60.02 Volume: 146.40 Matrix: 1.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 784 0 994 988 1464 N (int>3sigma) = 0 0 0 0 784 0 804 799 1185 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 54.8 57.2 55.9 Mean int/sigma = 0.0 0.0 0.0 0.0 18.7 0.0 22.1 23.1 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.107 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 105 335 N I>3s 10 10 28 335 0.9 0.9 0.7 28.5 5.6 5.6 3.2 22.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.224 1226 Fd-3m 1 1 227 C N N N N 37 2284 0.228 1264 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361403 8.368475 8.369053 90.0700 90.0089 90.0268 ZERR 1.00 0.000346 0.004388 0.001997 0.0024 0.0018 0.0146 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3401778- 667653 277 249 30 8.3 1055797.62 46.19 0.635 0.590 657245- 476804 196 183 30 6.1 513523.42 32.08 0.781 0.658 476264- 361201 225 210 30 7.0 362088.91 21.76 0.902 0.832 360917- 282234 172 144 30 4.8 220311.22 18.40 0.693 0.620 280290- 201402 179 160 30 5.3 202653.41 18.60 0.701 0.734 197052- 111686 184 160 30 5.3 123108.64 13.42 0.540 0.597 110567- 74095 160 148 30 4.9 91989.88 11.42 0.430 0.349 72549- 54125 92 85 30 2.8 63654.85 9.79 0.442 0.281 53043- 29344 72 65 30 2.2 39823.88 7.62 0.508 0.430 27676- 1346 63 60 30 2.0 7774.54 3.08 0.765 0.721 ------------------------------------------------------------------------------------------- 3401778- 1346 1620 1464 300 4.9 368056.01 22.48 0.694 0.632 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 316 287 30 9.6 684971.87 41.48 0.691 0.711 0.017 1.08-0.85 313 288 31 9.3 465391.38 23.87 0.785 0.719 0.027 0.83-0.73 229 212 30 7.1 374485.75 20.57 0.654 0.573 0.033 0.72-0.65 198 182 32 5.7 240153.17 16.62 0.723 0.696 0.040 0.65-0.60 163 144 33 4.4 231649.77 15.44 0.655 0.676 0.041 0.60-0.56 128 112 30 3.7 181969.32 13.88 0.535 0.460 0.047 0.56-0.52 106 90 30 3.0 154089.90 13.64 0.621 0.556 0.050 0.52-0.49 85 71 30 2.4 110899.03 10.89 0.397 0.286 0.056 0.49-0.45 53 49 30 1.6 143033.11 13.45 0.273 0.268 0.050 0.45-0.40 29 29 24 1.2 90580.10 10.82 0.385 0.385 0.058 ------------------------------------------------------------------------------------------------------ inf-0.40 1620 1464 300 4.9 368056.01 22.48 0.694 0.632 0.029 inf-0.60 1219 1113 156 7.1 437624.50 25.51 0.711 0.684 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 287 30 30 100.0 9.6 684971.87 139.42 0.691 0.007 1.08-0.85 288 31 31 100.0 9.3 465391.38 87.69 0.785 0.013 0.83-0.73 212 30 30 100.0 7.1 374485.75 67.40 0.654 0.016 0.72-0.65 182 32 32 100.0 5.7 240153.17 47.81 0.723 0.020 0.65-0.60 144 33 33 100.0 4.4 231649.77 40.56 0.655 0.025 0.60-0.56 112 35 30 85.7 3.7 181969.32 31.48 0.535 0.027 0.56-0.52 90 36 30 83.3 3.0 154089.90 29.41 0.621 0.033 0.52-0.49 71 48 30 62.5 2.4 110899.03 19.34 0.397 0.038 0.49-0.45 49 66 30 45.5 1.6 143033.11 18.07 0.273 0.039 0.45-0.40 29 119 24 20.2 1.2 90580.10 12.84 0.385 0.043 -------------------------------------------------------------------------------------------- inf-0.40 1464 462 300 64.9 4.9 368056.01 70.29 0.694 0.017 inf-0.60 1113 156 156 100.0 7.1 437624.50 84.55 0.711 0.013 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 -1.0 No constraint UB - matrix: 0.024835 -0.015540 -0.079548 ( 0.000009 0.000007 0.000009 ) -0.072566 0.032876 -0.029023 ( 0.000010 0.000007 0.000010 ) 0.036244 0.076561 -0.003570 ( 0.000007 0.000005 0.000007 ) M - matrix: 0.007196 0.000003 0.000001 ( 0.000002 0.000001 0.000001 ) 0.000003 0.007184 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000001 0.000009 0.007183 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.024835 -0.015540 -0.079548 ( 0.000009 0.000007 0.000009 ) -0.072566 0.032876 -0.029023 ( 0.000010 0.000007 0.000010 ) 0.036244 0.076561 -0.003570 ( 0.000007 0.000005 0.000007 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3614(9) 8.3686(6) 8.3691(9) 90.069(7) 90.009(8) 90.026(7) V = 585.60(10) unit cell: 8.3663(2) 8.3663(2) 8.3663(2) 90.0 90.0 90.0 V = 585.60(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.806) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.806) Run 3 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.806) PROFFIT INFO: signal sum: min=237.0000 max=20592796.0000 PROFFIT INFO: signal sum lp corr: min=585.8264 max=2947611.5937 PROFFIT INFO: background sum: min=1049.0000 max=26505.0000 PROFFIT INFO: background sum sig2: min=524.0000 max=12084.0000 PROFFIT INFO: num of signal pixels: min=51 max=520 PROFFIT INFO: Inet: min=937.3222 max=4716178.5000 PROFFIT INFO: sig(Inet): min=96.4556 max=47442.6602 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=229.72 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 16 102 294 652 720 1234 2112 2940 3242 Percent 0.0 0.0 0.5 3.1 9.1 20.1 22.2 38.1 65.1 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1621 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1621 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4716179- 1238071 162 1951891.10 125.78 100.00 1237685- 752787 162 957148.92 109.30 100.00 746269- 272705 162 481742.42 94.70 100.00 272160- 178378 162 213961.03 74.16 100.00 178076- 136588 162 158330.74 51.75 100.00 136516- 104448 162 117976.05 38.11 100.00 104317- 81451 162 92634.23 30.93 100.00 81125- 6119 162 49271.52 21.44 100.00 6112- 3334 162 4467.97 5.61 98.15 3331- 937 163 2480.16 4.28 70.55 ------------------------------------------------------------------------------------ 4716179- 937 1621 402743.34 55.57 96.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 162 752317.18 90.61 100.00 1.39- 1.09 162 813088.90 72.12 100.00 1.09- 0.96 162 363366.48 66.74 98.15 0.96- 0.85 162 433530.27 66.08 95.68 0.85- 0.80 162 472614.84 69.13 100.00 0.80- 0.73 162 263605.63 42.44 100.00 0.73- 0.70 162 247235.06 39.86 87.65 0.70- 0.65 162 315466.06 47.04 96.91 0.65- 0.62 162 187192.52 31.61 91.98 0.62- 0.58 163 180389.00 30.25 98.16 ------------------------------------------------------------------------------------ 4.82- 0.58 1621 402743.34 55.57 96.85 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:21:02 2018 Sorting 1621 observations 83 unique observations with > 7.00 F2/sig(F2) 1621 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 74 282 Total number of frames 282 Maximum number of 83 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1621 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 18 72 Total number of frames 72 1310 observations > 7.00 F2/sig(F2) 1310 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 18 72 Total number of frames 72 Removing 'redundancy=1' reflections Average redundancy: 14.5 (Out of 1310 removed 5 = 1305, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1305 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 18 72 Total number of frames 72 90 unique data precomputed (should be 90) 90 unique data with 1305 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 14.5 (Out of 1305 removed 0 = 1305, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 1305 observations RMS deviation of equivalent data = 0.13625 Rint = 0.11223 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11207, wR= 0.13946 Trying model 1 (ne=2, no=0)... Results: Rint= 0.06795, wR= 0.08708, Acormin=0.790, Acormax=1.292, Acor_av=1.012 F test: Probability=1.000, F= 2.709 Trying model 2 (ne=2, no=1)... Results: Rint= 0.06908, wR= 0.08603, Acormin=0.784, Acormax=1.311, Acor_av=0.987 F test: Probability=0.000, F= 0.965 Trying model 3 (ne=4, no=0)... Results: Rint= 0.05502, wR= 0.06949, Acormin=0.706, Acormax=1.319, Acor_av=0.959 F test: Probability=1.000, F= 1.514 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05272, wR= 0.06790, Acormin=0.701, Acormax=1.320, Acor_av=0.926 F test: Probability=0.924, F= 1.086 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04424, wR= 0.05816, Acormin=0.647, Acormax=1.305, Acor_av=0.911 F test: Probability=1.000, F= 1.533 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05215, wR= 0.06626, Acormin=0.702, Acormax=1.314, Acor_av=0.957 F test: Probability=0.000, F= 0.718 Trying model 7 (ne=6, no=1)... Results: Rint= 0.04988, wR= 0.06421, Acormin=0.707, Acormax=1.322, Acor_av=0.925 F test: Probability=0.000, F= 0.783 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04256, wR= 0.05505, Acormin=0.654, Acormax=1.333, Acor_av=0.929 F test: Probability=0.874, F= 1.069 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03315, wR= 0.04463, Acormin=0.612, Acormax=1.212, Acor_av=0.847 F test: Probability=1.000, F= 1.745 Trying model 10 (ne=8, no=0)... Results: Rint= 0.04678, wR= 0.06131, Acormin=0.657, Acormax=1.277, Acor_av=0.914 F test: Probability=0.000, F= 0.504 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04599, wR= 0.06048, Acormin=0.689, Acormax=1.270, Acor_av=0.892 F test: Probability=0.000, F= 0.520 Trying model 12 (ne=8, no=3)... Results: Rint= 0.03987, wR= 0.05107, Acormin=0.546, Acormax=1.089, Acor_av=0.775 F test: Probability=0.000, F= 0.688 Trying model 13 (ne=8, no=5)... Results: Rint= 0.02873, wR= 0.04076, Acormin=0.626, Acormax=1.192, Acor_av=0.832 F test: Probability=1.000, F= 1.312 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02725, wR= 0.03845, Acormin=0.626, Acormax=1.219, Acor_av=0.845 F test: Probability=0.941, F= 1.097 Final absorption model (ne=8, no=5): Rint= 0.02873, Acormin=0.626, Acormax=1.192, Acor_av=0.832 Combined refinement in use Rint: 0.11236 There are 72 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 5 (65 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13625 Using Levenberg-Marquardt: 0.00010 New wR= 0.03423 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11223 with corrections 0.02603 Rint for all data: 0.11236 with corrections 0.02626 4 observations identified as outliers and rejected Cycle 2 wR= 0.03154 Using Levenberg-Marquardt: 0.00001 New wR= 0.02967 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11176 with corrections 0.02271 Rint for all data: 0.11236 with corrections 0.02572 0 observations identified as outliers and rejected Cycle 3 wR= 0.02967 Using Levenberg-Marquardt: 0.00000 New wR= 0.02924 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11176 with corrections 0.02236 Rint for all data: 0.11236 with corrections 0.02544 0 observations identified as outliers and rejected Cycle 4 wR= 0.02924 Using Levenberg-Marquardt: 0.00000 New wR= 0.02900 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11176 with corrections 0.02211 Rint for all data: 0.11236 with corrections 0.02522 0 observations identified as outliers and rejected Cycle 5 wR= 0.02900 Using Levenberg-Marquardt: 0.00000 New wR= 0.02884 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11176 with corrections 0.02194 Rint for all data: 0.11236 with corrections 0.02506 0 observations identified as outliers and rejected Final wR= 0.02884 Final frame scales: Min= 0.8603 Max= 1.1289 Final absorption correction factors: Amin= 0.6694 Amax= 1.2731 PROFFIT INFO: Inet (after scale3 abspack): min=871.1797 max=5457346.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=108.8123 max=46865.3828 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1621 reflections read from tmp file 121 reflections are rejected (119 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 5 2 7 4 3 2 7 75 Initial Chi^2= 0.29838 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.43158 Current error model SIG(F2)^2 = 129.52*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 314.93*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 314.93*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5457346- 1227573 162 1956703.66 87.25 100.00 1221389- 727869 162 939856.08 39.98 100.00 727473- 290270 162 477294.10 39.22 100.00 290180- 176354 162 215060.18 27.70 100.00 176194- 142207 162 158516.77 19.52 100.00 141912- 102259 162 115046.76 13.91 100.00 101842- 80801 162 92392.65 11.81 100.00 80692- 5905 162 48960.81 8.40 91.98 5899- 3215 162 4306.77 3.03 19.75 3194- 871 163 2497.42 2.56 17.18 ------------------------------------------------------------------------------------ 5457346- 871 1621 400817.64 25.32 82.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 162 776240.20 58.47 96.30 1.39- 1.09 162 816216.41 45.37 91.98 1.09- 0.96 162 363021.15 26.02 83.33 0.96- 0.85 162 435096.63 25.10 84.57 0.85- 0.80 162 462923.10 25.76 89.51 0.80- 0.73 162 257897.44 16.10 72.22 0.73- 0.70 162 242007.46 15.14 77.78 0.70- 0.65 162 303930.97 17.64 86.42 0.65- 0.62 162 179058.13 12.11 75.93 0.62- 0.58 163 173190.06 11.62 70.55 ------------------------------------------------------------------------------------ 4.82- 0.58 1621 400817.64 25.32 82.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 162 776240.20 58.47 96.30 4.82- 1.09 324 796228.31 51.92 94.14 4.82- 0.96 486 651825.92 43.29 90.53 4.82- 0.85 648 597643.60 38.74 89.04 4.82- 0.80 810 570699.50 36.15 89.14 4.82- 0.73 972 518565.82 32.80 86.32 4.82- 0.70 1134 479057.48 30.28 85.10 4.82- 0.65 1296 457166.67 28.70 85.26 4.82- 0.62 1458 426265.72 26.86 84.22 4.82- 0.58 1621 400817.64 25.32 82.85 ------------------------------------------------------------------------------------ 4.82- 0.58 1621 400817.64 25.32 82.85 Scale applied to data: s=0.183239 (maximum obs:5457346.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.025; Rsigma 0.026: data 1621 -> merged 109 With outlier rejection... Rint 0.022; Rsigma 0.026: data 1613 -> merged 109 Rejected total: 8, method kkm 6, method Blessing 2 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585760, 4.830302 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 8.60 100.00 86 1.61 - 1.21 10 10 14.70 100.00 147 1.17 - 1.01 10 10 18.70 100.00 187 0.99 - 0.89 10 10 18.80 100.00 188 0.88 - 0.81 10 10 18.00 100.00 180 0.81 - 0.74 10 10 15.40 100.00 154 0.73 - 0.71 10 10 17.50 100.00 175 0.70 - 0.66 10 10 14.80 100.00 148 0.66 - 0.64 10 10 13.30 100.00 133 0.63 - 0.60 10 10 13.20 100.00 132 --------------------------------------------------------------- 5.91 - 0.60 100 100 15.30 100.00 1530 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:21:01 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914653 5.916290 5.915567 60.0592 90.0524 59.9835 1464 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.48 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 722 784 722 734 1114 988 1000 1464 N (int>3sigma) = 0 569 784 569 576 961 799 811 1185 Mean intensity = 0.0 48.3 24.4 48.2 55.1 39.9 57.2 54.7 55.9 Mean int/sigma = 0.0 20.9 18.7 20.9 22.1 20.1 23.1 22.6 22.5 Lattice type: P chosen Volume: 146.40 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Unitcell: 5.914 5.914 5.915 60.02 60.08 60.02 Niggli form: a.a = 34.970 b.b = 34.975 c.c = 34.983 b.c = 17.478 a.c = 17.446 a.b = 17.476 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.224 [ 1311] Vol = 585.6 Cell: 8.361 8.368 8.369 90.07 90.01 90.03 Volume: 585.60 Matrix: 1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.031 RHOMBOHEDRAL R-lattice R(int) = 0.190 [ 1060] Vol = 439.2 Cell: 5.916 5.921 14.482 90.01 89.97 120.02 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 2] err= 0.031 RHOMBOHEDRAL R-lattice R(int) = 0.171 [ 327] Vol = 439.2 Trigonal Cell: 5.916 5.921 14.482 90.01 89.97 120.02 Volume: 439.20 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.041 RHOMBOHEDRAL R-lattice R(int) = 0.217 [ 1041] Vol = 439.2 Cell: 5.914 5.916 14.498 89.94 90.07 120.01 Volume: 439.20 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.041 RHOMBOHEDRAL R-lattice R(int) = 0.202 [ 310] Vol = 439.2 Trigonal Cell: 5.914 5.916 14.498 89.94 90.07 120.01 Volume: 439.20 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.041 ORTHORHOMBIC I-lattice R(int) = 0.168 [ 1054] Vol = 292.8 Cell: 5.914 5.916 8.369 89.96 89.94 89.95 Volume: 292.80 Matrix:-1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.146 ORTHORHOMBIC I-lattice R(int) = 0.196 [ 1082] Vol = 292.8 Cell: 5.915 8.368 5.916 90.03 89.95 90.07 Volume: 292.80 Matrix: 1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.031 MONOCLINIC I-lattice R(int) = 0.168 [ 854] Vol = 292.8 Cell: 5.915 5.916 8.368 89.97 90.07 90.05 Volume: 292.80 Matrix: 1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.033 MONOCLINIC I-lattice R(int) = 0.158 [ 814] Vol = 292.8 Cell: 5.914 5.916 8.369 90.04 90.06 89.95 Volume: 292.80 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.040 MONOCLINIC I-lattice R(int) = 0.152 [ 775] Vol = 292.8 Cell: 5.916 5.914 8.369 90.06 90.04 89.95 Volume: 292.80 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.052 MONOCLINIC I-lattice R(int) = 0.152 [ 775] Vol = 292.8 Cell: 8.369 5.914 5.916 89.95 90.04 90.06 Volume: 292.80 Matrix: 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [31] err= 0.000 TRICLINIC P-lattice R(int) = 0.114 [ 474] Vol = 146.4 Cell: 5.914 5.914 5.915 60.02 60.08 60.02 Volume: 146.40 Matrix: 1.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 784 0 994 988 1464 N (int>3sigma) = 0 0 0 0 784 0 804 799 1185 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 54.8 57.2 55.9 Mean int/sigma = 0.0 0.0 0.0 0.0 18.7 0.0 22.1 23.1 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.107 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 15 15 105 335 N I>3s 10 10 28 335 0.9 0.9 0.7 28.5 5.6 5.6 3.2 22.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.224 1226 Fd-3m 1 1 227 C N N N N 37 2284 0.228 1264 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361403 8.368475 8.369053 90.0700 90.0089 90.0268 ZERR 1.00 0.000346 0.004388 0.001997 0.0024 0.0018 0.0146 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4540360- 594461 363 360 27 13.3 1344586.53 58.95 0.019 0.021 592836- 133183 473 470 27 17.4 240883.32 27.83 0.025 0.028 122000- 39828 412 412 27 15.3 91363.75 11.73 0.037 0.046 11486- 2098 373 371 28 13.3 4017.99 2.97 0.140 0.171 ------------------------------------------------------------------------------------------- 4540360- 2098 1621 1613 109 14.8 394543.61 24.94 0.022 0.024 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 395 388 27 14.4 686559.37 46.25 0.021 0.021 0.015 1.01-0.78 481 480 27 17.8 388728.16 23.01 0.017 0.021 0.026 0.78-0.65 429 429 28 15.3 294280.54 17.29 0.023 0.028 0.038 0.65-0.59 316 316 27 11.7 180942.86 12.11 0.036 0.038 0.053 ------------------------------------------------------------------------------------------------------ inf-0.59 1621 1613 109 14.8 394543.61 24.94 0.022 0.024 0.026 inf-0.60 1536 1528 99 15.4 408871.44 25.74 0.021 0.024 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 388 27 27 100.0 14.4 686559.37 184.27 0.021 0.004 1.01-0.78 480 27 27 100.0 17.8 388728.16 101.36 0.017 0.006 0.78-0.65 429 28 28 100.0 15.3 294280.54 72.40 0.023 0.011 0.65-0.59 316 28 27 96.4 11.7 180942.86 46.48 0.036 0.018 -------------------------------------------------------------------------------------------- inf-0.59 1613 110 109 99.1 14.8 394543.61 102.85 0.022 0.007 inf-0.60 1528 99 99 100.0 15.4 408871.44 106.53 0.021 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:27:57 2018) ID: 2932; threads 39; handles 878; mem 518192.00 (1237700.00)kB; time: 1w 4d 23h 33m 28s MEMORY INFO: Memory PF:0.0, Ph:218.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.0,peak PF: 697.1, WS: 297.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:218.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.8,peak PF: 697.1, WS: 299.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:27:57 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000018 0.000014 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000011 0.000011 ) 5.91502 ( 0.00092 ) 5.91640 ( 0.00092 ) 5.92265 ( 0.00074 ) 60.05206 ( 0.01465 ) 89.98756 ( 0.01134 ) 60.01743 ( 0.01631 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:27:58 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000018 0.000014 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000011 0.000011 ) M - matrix: 0.021590 -0.014392 0.007204 ( 0.000005 0.000003 0.000003 ) -0.014392 0.028736 -0.014357 ( 0.000003 0.000004 0.000003 ) 0.007204 -0.014357 0.021550 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9150(9) 5.9164(9) 5.9227(7) 60.052(15) 89.988(11) 60.017(16) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb PROFFITPEAK info: 1295 peaks in the peak location table UB fit with 550 obs out of 593 (total:593,skipped:0) (92.75%) UB - matrix: -0.069866 0.031072 0.088907 ( 0.000057 0.000055 0.000070 ) -0.068957 -0.065588 -0.010253 ( 0.000049 0.000048 0.000060 ) 0.109079 -0.152860 0.116074 ( 0.000066 0.000065 0.000082 ) M - matrix: 0.021535 -0.014322 0.007157 ( 0.000018 0.000014 0.000014 ) -0.014322 0.028633 -0.014308 ( 0.000014 0.000021 0.000016 ) 0.007157 -0.014308 0.021483 ( 0.000014 0.000016 0.000023 ) unit cell: 5.917(3) 5.924(3) 5.925(3) 60.02(6) 90.00(4) 60.03(6) V = 146.94(12) UB fit with 550 obs out of 593 (total:593,skipped:0) (92.75%) UB - matrix: -0.069866 0.031072 0.088907 ( 0.000057 0.000055 0.000070 ) -0.068957 -0.065588 -0.010253 ( 0.000049 0.000048 0.000060 ) 0.109079 -0.152860 0.116074 ( 0.000066 0.000065 0.000082 ) M - matrix: 0.021535 -0.014322 0.007157 ( 0.000018 0.000014 0.000014 ) -0.014322 0.028633 -0.014308 ( 0.000014 0.000021 0.000016 ) 0.007157 -0.014308 0.021483 ( 0.000014 0.000016 0.000023 ) unit cell: 5.917(3) 5.924(3) 5.925(3) 60.02(6) 90.00(4) 60.03(6) V = 146.94(12) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.069898 0.031094 0.088811 ( 0.000055 0.000054 0.000068 ) -0.068906 -0.065687 -0.010265 ( 0.000051 0.000050 0.000063 ) 0.108978 -0.152697 0.116093 ( 0.000064 0.000062 0.000079 ) M - matrix: 0.021510 -0.014288 0.007151 ( 0.000017 0.000013 0.000014 ) -0.014288 0.028598 -0.014291 ( 0.000013 0.000020 0.000016 ) 0.007151 -0.014291 0.021470 ( 0.000014 0.000016 0.000022 ) UB fit with 554 obs out of 593 (total:593,skipped:0) (93.42%) unit cell: 5.917(3) 5.923(3) 5.926(3) 60.03(6) 90.05(4) 60.09(6) V = 147.05(12) UB fit with 554 obs out of 593 (total:593,skipped:0) (93.42%) UB - matrix: -0.069898 0.031094 0.088811 ( 0.000055 0.000054 0.000068 ) -0.068906 -0.065687 -0.010266 ( 0.000051 0.000050 0.000063 ) 0.108978 -0.152697 0.116093 ( 0.000064 0.000062 0.000079 ) M - matrix: 0.021510 -0.014288 0.007151 ( 0.000017 0.000013 0.000014 ) -0.014288 0.028598 -0.014291 ( 0.000013 0.000020 0.000016 ) 0.007151 -0.014291 0.021470 ( 0.000014 0.000016 0.000022 ) unit cell: 5.917(3) 5.923(3) 5.926(3) 60.03(6) 90.05(4) 60.09(6) V = 147.05(12) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 593 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Run 3 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 749 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069898 0.031094 0.088811 ( 0.000055 0.000054 0.000068 ) -0.068906 -0.065687 -0.010266 ( 0.000051 0.000050 0.000063 ) 0.108978 -0.152697 0.116093 ( 0.000064 0.000062 0.000079 ) M - matrix: 0.021510 -0.014288 0.007151 ( 0.000017 0.000013 0.000014 ) -0.014288 0.028598 -0.014291 ( 0.000013 0.000020 0.000016 ) 0.007151 -0.014291 0.021470 ( 0.000014 0.000016 0.000022 ) UB fit with 554 obs out of 593 (total:593,skipped:0) (93.42%) unit cell: 5.917(3) 5.923(3) 5.926(3) 60.03(6) 90.05(4) 60.09(6) V = 147.05(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 555 obs out of 593 (total:593,skipped:0) (93.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb 7 of 447 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 44 | 0.993 ( 0.127) | 1.104 ( 0.428) | 1.091 ( 0.597) | 1.41- 1.17 | 44 | 1.040 ( 0.127) | 1.178 ( 0.490) | 0.996 ( 0.515) | 1.17- 0.99 | 44 | 0.995 ( 0.093) | 1.041 ( 0.269) | 1.014 ( 0.438) | 0.99- 0.92 | 44 | 1.024 ( 0.075) | 1.021 ( 0.098) | 1.127 ( 0.447) | 0.91- 0.82 | 44 | 1.002 ( 0.086) | 0.982 ( 0.112) | 1.121 ( 0.409) | 0.82- 0.75 | 44 | 0.989 ( 0.082) | 0.947 ( 0.100) | 1.095 ( 0.446) | 0.75- 0.71 | 44 | 0.978 ( 0.042) | 0.910 ( 0.060) | 1.253 ( 0.505) | 0.71- 0.66 | 44 | 0.950 ( 0.051) | 0.856 ( 0.053) | 1.245 ( 0.492) | 0.66- 0.62 | 44 | 0.929 ( 0.045) | 0.836 ( 0.035) | 1.199 ( 0.432) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.811 ( 0.039) | 1.304 ( 0.560) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 440 | 0.980 ( 0.092) | 0.968 ( 0.258) | 1.145 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) UB - matrix: -0.069974 0.031022 0.089001 ( 0.000029 0.000027 0.000033 ) -0.068564 -0.066028 -0.010156 ( 0.000020 0.000018 0.000023 ) 0.108971 -0.152891 0.116296 ( 0.000022 0.000020 0.000025 ) M - matrix: 0.021472 -0.014304 0.007141 ( 0.000007 0.000005 0.000005 ) -0.014304 0.028698 -0.014349 ( 0.000005 0.000007 0.000005 ) 0.007141 -0.014349 0.021549 ( 0.000005 0.000005 0.000008 ) unit cell: 5.9228(13) 5.9169(12) 5.9161(15) 59.98(2) 89.957(19) 60.05(2) V = 146.71(5) OTKP changes: 440 1 1 1 UB - matrix: -0.069865 0.030977 0.088998 ( 0.000027 0.000025 0.000030 ) -0.068794 -0.065797 -0.010220 ( 0.000016 0.000015 0.000019 ) 0.109158 -0.152979 0.116326 ( 0.000022 0.000020 0.000025 ) M - matrix: 0.021529 -0.014337 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014337 0.028692 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014366 0.021557 ( 0.000005 0.000005 0.000008 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 5.9179(11) 5.9207(11) 5.9183(14) 59.98(2) 90.018(17) 60.047(19) V = 146.66(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.906) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069865 0.030977 0.088998 ( 0.000027 0.000025 0.000030 ) -0.068794 -0.065797 -0.010220 ( 0.000016 0.000015 0.000019 ) 0.109158 -0.152979 0.116326 ( 0.000022 0.000020 0.000025 ) M - matrix: 0.021529 -0.014337 0.007183 ( 0.000006 0.000005 0.000005 ) -0.014337 0.028692 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007183 -0.014366 0.021557 ( 0.000005 0.000005 0.000008 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 5.9179(11) 5.9207(11) 5.9183(14) 59.98(2) 90.018(17) 60.047(19) V = 146.66(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 44 | 1.020 ( 0.243) | 1.200 ( 0.666) | 1.114 ( 0.619) | 1.41- 1.17 | 44 | 1.023 ( 0.086) | 1.070 ( 0.183) | 0.951 ( 0.365) | 1.17- 1.01 | 44 | 0.990 ( 0.095) | 1.076 ( 0.381) | 1.002 ( 0.459) | 0.99- 0.92 | 44 | 1.031 ( 0.069) | 1.035 ( 0.100) | 1.117 ( 0.439) | 0.92- 0.82 | 44 | 1.000 ( 0.082) | 0.972 ( 0.104) | 1.137 ( 0.385) | 0.82- 0.75 | 44 | 0.990 ( 0.082) | 0.950 ( 0.103) | 1.107 ( 0.451) | 0.75- 0.71 | 44 | 0.985 ( 0.045) | 0.923 ( 0.070) | 1.224 ( 0.483) | 0.71- 0.67 | 44 | 0.951 ( 0.050) | 0.856 ( 0.053) | 1.225 ( 0.490) | 0.67- 0.62 | 44 | 0.936 ( 0.048) | 0.842 ( 0.037) | 1.189 ( 0.433) | 0.62- 0.59 | 47 | 0.903 ( 0.043) | 0.811 ( 0.038) | 1.354 ( 0.568) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 443 | 0.982 ( 0.108) | 0.972 ( 0.282) | 1.143 ( 0.488) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.4 | 129 | 1.118 ( 0.119) | 1.259 ( 0.479) | 1.139 ( 0.541) | 13.4-19.2 | 129 | 1.078 ( 0.057) | 1.126 ( 0.248) | 1.212 ( 0.535) | 19.3-23.4 | 129 | 1.075 ( 0.080) | 1.144 ( 0.377) | 1.165 ( 0.488) | 23.4-27.4 | 129 | 1.035 ( 0.085) | 1.086 ( 0.327) | 1.235 ( 0.594) | 27.4-31.0 | 129 | 1.019 ( 0.083) | 1.003 ( 0.187) | 1.250 ( 0.498) | 31.0-34.0 | 129 | 0.980 ( 0.090) | 0.923 ( 0.102) | 1.203 ( 0.512) | 34.0-37.0 | 130 | 0.967 ( 0.081) | 0.892 ( 0.092) | 1.216 ( 0.508) | 37.0-39.8 | 129 | 0.949 ( 0.099) | 0.884 ( 0.161) | 1.171 ( 0.560) | 39.8-42.9 | 129 | 0.928 ( 0.091) | 0.839 ( 0.090) | 1.179 ( 0.509) | 42.9-49.9 | 128 | 0.936 ( 0.087) | 0.816 ( 0.069) | 1.170 ( 0.454) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1290 | 1.008 ( 0.109) | 0.997 ( 0.289) | 1.194 ( 0.522) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0098 b=1.27 e3 dimension: a=0.0029 b=0.98 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 23928508 lp-corr: 2786584 PROFFITPEAK - Finished at Tue Mar 27 14:28:16 2018 PROFFITMAIN - Started at Tue Mar 27 14:28:16 2018 OTKP changes: 1290 2 3 3 OTKP changes: 1290 2 3 3 UB - matrix: -0.070211 0.031077 0.088920 ( 0.000017 0.000014 0.000014 ) -0.068761 -0.065832 -0.010545 ( 0.000017 0.000014 0.000013 ) 0.109223 -0.153080 0.116344 ( 0.000014 0.000012 0.000011 ) M - matrix: 0.021587 -0.014375 0.007190 ( 0.000004 0.000003 0.000003 ) -0.014375 0.028733 -0.014352 ( 0.000003 0.000004 0.000003 ) 0.007190 -0.014352 0.021554 ( 0.000003 0.000003 0.000004 ) UB fit with 1290 obs out of 1290 (total:1290,skipped:0) (100.00%) unit cell: 5.9118(9) 5.9138(9) 5.9140(7) 60.052(14) 90.036(11) 60.012(15) V = 146.30(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070063 0.030674 0.088946 ( 0.000028 0.000028 0.000016 ) -0.068232 -0.066135 -0.010527 ( 0.000025 0.000025 0.000014 ) 0.109081 -0.153066 0.115995 ( 0.000025 0.000024 0.000014 ) M - matrix: 0.021463 -0.014333 0.007139 ( 0.000007 0.000006 0.000004 ) -0.014333 0.028744 -0.014330 ( 0.000006 0.000008 0.000004 ) 0.007139 -0.014330 0.021477 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9282(14) 5.9139(14) 5.9247(11) 60.02(2) 89.974(18) 59.99(2) V = 146.94(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070334 0.030944 0.088803 ( 0.000026 0.000026 0.000015 ) -0.068413 -0.066133 -0.010684 ( 0.000024 0.000023 0.000013 ) 0.109336 -0.153290 0.116374 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021582 -0.014412 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028829 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014385 0.021543 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9072(13) 5.9179(10) 60.05(2) 90.071(16) 60.00(2) V = 146.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.789) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070334 0.030944 0.088803 ( 0.000026 0.000026 0.000015 ) -0.068413 -0.066133 -0.010684 ( 0.000024 0.000023 0.000013 ) 0.109336 -0.153290 0.116374 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021582 -0.014412 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028829 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014385 0.021543 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9072(13) 5.9179(10) 60.05(2) 90.071(16) 60.00(2) V = 146.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070334 0.030944 0.088803 ( 0.000026 0.000026 0.000015 ) -0.068413 -0.066133 -0.010684 ( 0.000024 0.000023 0.000013 ) 0.109336 -0.153290 0.116374 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021582 -0.014412 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028829 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014385 0.021543 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9156(13) 5.9072(13) 5.9179(10) 60.05(2) 90.071(16) 60.00(2) V = 146.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070408 0.031336 0.088627 ( 0.000025 0.000022 0.000027 ) -0.068585 -0.065986 -0.010254 ( 0.000031 0.000027 0.000033 ) 0.108997 -0.152676 0.116254 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021542 -0.014322 0.007135 ( 0.000007 0.000005 0.000005 ) -0.014322 0.028646 -0.014295 ( 0.000005 0.000006 0.000005 ) 0.007135 -0.014295 0.021475 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(16) 5.9211(16) 5.9230(13) 60.02(3) 89.95(2) 60.01(3) V = 146.81(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070360 0.031207 0.088848 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065856 -0.010351 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153159 0.116583 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021601 -0.014385 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014385 0.028768 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014401 0.021593 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9093(16) 5.9162(16) 5.9143(12) 59.94(2) 89.947(19) 60.01(3) V = 146.15(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.789) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070360 0.031207 0.088848 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065856 -0.010351 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153159 0.116583 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021601 -0.014385 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014385 0.028768 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014401 0.021593 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9093(16) 5.9162(16) 5.9143(12) 59.94(2) 89.947(19) 60.01(3) V = 146.15(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070360 0.031207 0.088848 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065856 -0.010351 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153159 0.116583 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021601 -0.014385 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014385 0.028768 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014401 0.021593 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9093(16) 5.9162(16) 5.9143(12) 59.94(2) 89.947(19) 60.01(3) V = 146.15(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.069967 0.030971 0.089026 ( 0.000028 0.000026 0.000032 ) -0.068691 -0.065979 -0.010232 ( 0.000018 0.000017 0.000020 ) 0.109077 -0.152951 0.116337 ( 0.000023 0.000022 0.000027 ) M - matrix: 0.021512 -0.014318 0.007164 ( 0.000007 0.000005 0.000005 ) -0.014318 0.028706 -0.014361 ( 0.000005 0.000007 0.000006 ) 0.007164 -0.014361 0.021565 ( 0.000005 0.000006 0.000008 ) unit cell: 5.9170(12) 5.9155(12) 5.9150(15) 59.98(2) 90.002(19) 60.07(2) V = 146.52(5) OTKP changes: 443 1 1 1 UB - matrix: -0.069860 0.030973 0.089007 ( 0.000028 0.000026 0.000032 ) -0.068771 -0.065816 -0.010212 ( 0.000016 0.000015 0.000019 ) 0.109148 -0.152972 0.116333 ( 0.000024 0.000022 0.000027 ) M - matrix: 0.021523 -0.014334 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014334 0.028691 -0.014367 ( 0.000005 0.000007 0.000006 ) 0.007182 -0.014367 0.021560 ( 0.000005 0.000006 0.000008 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9187(12) 5.9207(11) 5.9178(14) 59.98(2) 90.017(18) 60.05(2) V = 146.67(5) Run 3 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069860 0.030973 0.089007 ( 0.000028 0.000026 0.000032 ) -0.068771 -0.065816 -0.010212 ( 0.000016 0.000015 0.000019 ) 0.109148 -0.152972 0.116333 ( 0.000024 0.000022 0.000027 ) M - matrix: 0.021523 -0.014334 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014334 0.028691 -0.014367 ( 0.000005 0.000007 0.000006 ) 0.007182 -0.014367 0.021560 ( 0.000005 0.000006 0.000008 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9187(12) 5.9207(11) 5.9178(14) 59.98(2) 90.017(18) 60.05(2) V = 146.67(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.069860 0.030973 0.089007 ( 0.000028 0.000026 0.000032 ) -0.068771 -0.065816 -0.010212 ( 0.000016 0.000015 0.000019 ) 0.109148 -0.152972 0.116333 ( 0.000024 0.000022 0.000027 ) M - matrix: 0.021523 -0.014334 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014334 0.028691 -0.014367 ( 0.000005 0.000007 0.000006 ) 0.007182 -0.014367 0.021560 ( 0.000005 0.000006 0.000008 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9187(12) 5.9207(11) 5.9178(14) 59.98(2) 90.017(18) 60.05(2) V = 146.67(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070181 0.031076 0.088855 ( 0.000017 0.000014 0.000014 ) -0.068756 -0.065723 -0.010607 ( 0.000019 0.000015 0.000015 ) 0.109181 -0.153059 0.116373 ( 0.000014 0.000011 0.000011 ) M - matrix: 0.021573 -0.014373 0.007199 ( 0.000005 0.000003 0.000003 ) -0.014373 0.028712 -0.014354 ( 0.000003 0.000004 0.000003 ) 0.007199 -0.014354 0.021550 ( 0.000003 0.000003 0.000004 ) UB fit with 1290 obs out of 1290 (total:1290,skipped:0) (100.00%) unit cell: 5.9153(9) 5.9178(9) 5.9160(7) 60.048(15) 90.055(11) 60.006(17) V = 146.49(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 59 reflections under beam stop or inside a detector rejection region 13 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof 1768 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:28:20 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.789) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.789) Run 3 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) PROFFIT INFO: signal sum: min=237.0000 max=20618772.0000 PROFFIT INFO: signal sum lp corr: min=577.5404 max=2944722.9351 PROFFIT INFO: background sum: min=704.0000 max=26070.0000 PROFFIT INFO: background sum sig2: min=525.0000 max=12359.0000 PROFFIT INFO: num of signal pixels: min=49 max=555 PROFFIT INFO: Inet: min=924.0646 max=4711557.0000 PROFFIT INFO: sig(Inet): min=128.1861 max=47452.1914 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.75 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 10 64 163 358 396 681 1157 1603 1768 Percent 0.0 0.0 0.6 3.6 9.2 20.2 22.4 38.5 65.4 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1768 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1768 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711557- 1234325 176 1945900.41 125.79 100.00 1231453- 740329 176 949150.62 108.75 100.00 739556- 276104 176 476459.53 95.22 100.00 275832- 177543 176 214695.43 74.73 100.00 177369- 135693 176 157893.40 51.76 100.00 134537- 104082 176 117934.44 38.13 100.00 104081- 80032 176 91550.64 30.73 100.00 80018- 6122 176 48098.21 21.34 100.00 6116- 3329 176 4439.96 5.71 98.30 3327- 924 184 2461.16 4.08 66.85 ------------------------------------------------------------------------------------ 4711557- 924 1768 399055.68 55.39 96.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 176 713866.65 86.67 98.86 1.32- 1.05 176 589387.17 69.24 97.73 1.05- 0.92 176 493181.90 64.14 98.30 0.92- 0.82 176 358966.53 54.22 94.89 0.82- 0.74 176 422445.78 58.92 96.59 0.74- 0.67 176 389340.02 55.32 96.59 0.67- 0.62 176 282483.60 46.64 96.59 0.62- 0.57 176 309900.22 47.14 93.18 0.57- 0.52 176 238305.33 39.25 96.59 0.52- 0.40 184 201652.45 33.38 94.57 ------------------------------------------------------------------------------------ 5.26- 0.40 1768 399055.68 55.39 96.38 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:28:20 2018 Sorting 1768 observations 234 unique observations with > 7.00 F2/sig(F2) 1768 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 99 307 Total number of frames 307 Maximum number of 234 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1768 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 49 155 Total number of frames 155 1428 observations > 7.00 F2/sig(F2) 1428 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 49 155 Total number of frames 155 Removing 'redundancy=1' reflections Average redundancy: 6.0 (Out of 1428 removed 51 = 1377, unique = 228) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1377 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 49 155 Total number of frames 155 228 unique data precomputed (should be 228) 228 unique data with 1377 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.0 (Out of 1377 removed 0 = 1377, unique = 228) 228 unique data precomputed (should be 228) 228 unique data with 1377 observations RMS deviation of equivalent data = 0.70109 Rint = 0.66778 10 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.64289, wR= 3.72245 Trying model 1 (ne=2, no=0)... Results: Rint= 0.71210, wR= 2.65775, Acormin=-0.006, Acormax=2.092, Acor_av=0.632 F test: Probability=0.000, F= 0.811 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88695, wR= 2.78046, Acormin=-0.349, Acormax=1.862, Acor_av=0.351 F test: Probability=0.000, F= 0.522 Trying model 3 (ne=4, no=0)... Results: Rint= 0.74139, wR= 2.16664, Acormin=-0.114, Acormax=2.190, Acor_av=0.508 F test: Probability=0.000, F= 0.743 Trying model 4 (ne=4, no=1)... Results: Rint= 0.89042, wR= 2.36454, Acormin=-0.529, Acormax=1.990, Acor_av=0.284 F test: Probability=0.000, F= 0.514 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96170, wR= 2.11008, Acormin=-1.106, Acormax=1.455, Acor_av=0.083 F test: Probability=0.000, F= 0.437 Trying model 6 (ne=6, no=0)... Results: Rint= 0.78291, wR= 2.26818, Acormin=-0.211, Acormax=2.764, Acor_av=0.435 F test: Probability=0.000, F= 0.658 Trying model 7 (ne=6, no=1)... Results: Rint= 0.92064, wR= 2.54625, Acormin=-0.621, Acormax=2.230, Acor_av=0.209 F test: Probability=0.000, F= 0.475 Trying model 8 (ne=6, no=3)... Results: Rint= 0.96490, wR= 2.50200, Acormin=-1.166, Acormax=1.487, Acor_av=0.067 F test: Probability=0.000, F= 0.430 Trying model 9 (ne=6, no=5)... Results: Rint= 1.01570, wR= 2.18337, Acormin=-0.507, Acormax=1.898, Acor_av=0.010 F test: Probability=0.000, F= 0.384 Trying model 10 (ne=8, no=0)... Results: Rint= 0.84981, wR= 1.88342, Acormin=-0.606, Acormax=3.220, Acor_av=0.325 F test: Probability=0.000, F= 0.550 Trying model 11 (ne=8, no=1)... Results: Rint= 1.02035, wR= 2.05004, Acormin=-1.022, Acormax=1.355, Acor_av=0.030 F test: Probability=0.000, F= 0.381 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97845, wR= 1.34867, Acormin=-0.043, Acormax=0.080, Acor_av=0.002 F test: Probability=0.000, F= 0.411 Trying model 13 (ne=8, no=5)... Results: Rint= 0.97780, wR= 1.35712, Acormin=-0.042, Acormax=0.082, Acor_av=0.002 F test: Probability=0.000, F= 0.408 Trying model 14 (ne=8, no=7)... Results: Rint= 0.98701, wR= 1.49239, Acormin=-0.051, Acormax=0.078, Acor_av=0.001 F test: Probability=0.000, F= 0.394 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.83600 There are 155 active scales (one needs to be fixed) Refinement control: frame scale #137 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.70109 Using Levenberg-Marquardt: 0.00010 New wR= 0.68127 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66778 with corrections 0.64487 Rint for all data: 0.83600 with corrections 0.81745 10 observations identified as outliers and rejected Cycle 2 wR= 0.64120 Using Levenberg-Marquardt: 0.00001 New wR= 0.64983 Using Levenberg-Marquardt: 0.00010 New wR= 0.64762 Using Levenberg-Marquardt: 0.00100 New wR= 0.63974 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64289 with corrections 0.62231 Rint for all data: 0.83600 with corrections 0.81984 5 observations identified as outliers and rejected Cycle 3 wR= 0.61853 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61243 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63443 with corrections 0.62744 Rint for all data: 0.83600 with corrections 0.82971 4 observations identified as outliers and rejected Cycle 4 wR= 0.60870 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60708 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63280 with corrections 0.62364 Rint for all data: 0.83600 with corrections 0.82825 5 observations identified as outliers and rejected Cycle 5 wR= 0.60145 Using Levenberg-Marquardt: 0.01000 New wR= 0.63653 Using Levenberg-Marquardt: 0.10000 New wR= 0.60059 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62949 with corrections 0.62483 Rint for all data: 0.83600 with corrections 0.83138 1 observations identified as outliers and rejected Final wR= 0.60059 Final frame scales: Min= 0.5018 Max= 2.4553 Final absorption correction factors: Amin= 0.3438 Amax= 1.8061 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=641.4488 max=6220503.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=125.4981 max=82531.3906 PROFFIT INFO: 14 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/109 1754 reflections read from tmp file 1360 reflections are rejected (1261 as outliers, 99 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 80 41 11 8 2 1 1 Initial Chi^2= 0.79220 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.22739 Current error model SIG(F2)^2 = 298.08*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 365.86*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 365.86*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6220504- 1219602 175 2118718.64 76.41 100.00 1218874- 592567 175 886131.44 40.95 100.00 590490- 292313 175 417577.95 34.43 100.00 292289- 187725 175 235217.34 25.74 100.00 186418- 131603 175 156788.29 17.45 100.00 131544- 96247 175 113142.94 14.52 100.00 95953- 59250 175 76272.67 11.58 100.00 58982- 6465 175 36234.31 8.45 88.00 6430- 2939 175 4133.15 2.84 21.14 2908- 641 179 2129.69 2.24 6.70 ------------------------------------------------------------------------------------ 6220504- 641 1754 403716.73 23.41 81.41 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 175 958497.86 51.12 94.86 1.32- 1.05 175 615178.67 34.19 88.57 1.05- 0.92 175 558804.34 27.50 85.14 0.92- 0.82 175 365745.27 21.06 77.71 0.82- 0.74 175 424864.73 22.40 83.43 0.74- 0.67 175 345079.07 19.73 76.57 0.67- 0.62 175 237116.70 16.07 77.71 0.62- 0.57 175 258655.42 16.79 81.14 0.57- 0.52 175 164901.00 13.73 78.86 0.52- 0.40 179 114925.16 11.80 70.39 ------------------------------------------------------------------------------------ 5.26- 0.40 1754 403716.73 23.41 81.41 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 175 958497.86 51.12 94.86 5.26- 1.05 350 786838.27 42.65 91.71 5.26- 0.92 525 710826.96 37.60 89.52 5.26- 0.82 700 624556.54 33.47 86.57 5.26- 0.74 875 584618.18 31.25 85.94 5.26- 0.67 1050 544694.99 29.33 84.38 5.26- 0.62 1225 500755.24 27.44 83.43 5.26- 0.57 1400 470492.76 26.11 83.14 5.26- 0.52 1575 436538.12 24.73 82.67 5.26- 0.40 1754 403716.73 23.41 81.41 ------------------------------------------------------------------------------------ 5.26- 0.40 1754 403716.73 23.41 81.41 Scale applied to data: s=0.160759 (maximum obs:6220503.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.828; Rsigma 0.027: data 1754 -> merged 301 With outlier rejection... Rint 0.716; Rsigma 0.028: data 1587 -> merged 301 Rejected total: 167, method kkm 156, method Blessing 11 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404305, 5.271498 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 7.47 100.00 112 1.46 - 1.12 15 15 12.27 100.00 184 1.08 - 0.96 15 15 10.47 100.00 157 0.96 - 0.86 15 15 9.67 100.00 145 0.86 - 0.79 15 15 8.27 100.00 124 0.79 - 0.73 15 15 7.27 100.00 109 0.73 - 0.69 15 15 6.47 100.00 97 0.69 - 0.65 15 15 6.73 100.00 101 0.65 - 0.63 15 15 4.33 100.00 65 0.63 - 0.60 21 21 4.52 100.00 95 --------------------------------------------------------------- 5.92 - 0.60 156 156 7.62 100.00 1189 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:28:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915330 5.917811 5.915996 60.0481 90.0549 60.0064 1587 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 773 842 789 801 1202 1061 1067 1587 N (int>3sigma) = 0 608 842 624 628 1037 864 866 1285 Mean intensity = 0.0 50.2 25.6 49.9 56.8 41.5 60.3 58.3 58.8 Mean int/sigma = 0.0 20.8 18.6 20.8 21.6 20.0 23.3 22.8 22.5 Lattice type: P chosen Volume: 146.49 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.915 5.915 5.916 90.05 119.98 119.93 Niggli form: a.a = 34.986 b.b = 34.991 c.c = 34.999 b.c = -0.034 a.c = -17.486 a.b = -17.458 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.107 CUBIC F-lattice R(int) = 0.245 [ 1434] Vol = 586.0 Cell: 8.370 8.372 8.362 90.03 89.99 89.96 Volume: 585.95 Matrix:-1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.088 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 1171] Vol = 439.5 Cell: 5.921 5.915 14.493 90.02 90.02 120.04 Volume: 439.46 Matrix: 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.088 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 353] Vol = 439.5 Trigonal Cell: 5.921 5.915 14.493 90.02 90.02 120.04 Volume: 439.46 Matrix: 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.025 TETRAGONAL I-lattice R(int) = 0.187 [ 1198] Vol = 293.0 Cell: 5.917 5.921 8.362 89.98 89.98 89.99 Volume: 292.98 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.037 TETRAGONAL I-lattice R(int) = 0.187 [ 1198] Vol = 293.0 Cell: 5.921 5.917 8.362 90.02 90.02 89.99 Volume: 292.98 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.185 [ 1153] Vol = 293.0 Cell: 5.921 5.917 8.362 89.98 89.98 89.99 Volume: 292.98 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.193 [ 1168] Vol = 293.0 Cell: 5.915 8.370 5.918 90.02 89.93 90.03 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.137 [ 939] Vol = 293.0 Cell: 5.917 5.921 8.362 90.02 90.02 89.99 Volume: 292.98 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.043 MONOCLINIC I-lattice R(int) = 0.176 [ 912] Vol = 293.0 Cell: 5.915 5.918 8.370 89.98 90.03 90.07 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.027 MONOCLINIC I-lattice R(int) = 0.146 [ 909] Vol = 293.0 Cell: 5.915 8.370 5.918 90.02 90.07 89.97 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.081 MONOCLINIC C-lattice R(int) = 0.166 [ 941] Vol = 293.0 Cell: 10.252 5.915 5.916 90.05 125.25 89.93 Volume: 292.98 Matrix: 1.0000 -2.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.111 [ 579] Vol = 146.5 Cell: 5.915 5.915 5.916 90.05 119.98 119.93 Volume: 146.49 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 842 0 1055 1070 1587 N (int>3sigma) = 0 0 0 0 842 0 858 867 1285 Mean intensity = 0.0 0.0 0.0 0.0 25.6 0.0 59.0 59.0 58.8 Mean int/sigma = 0.0 0.0 0.0 0.0 18.6 0.0 22.5 22.5 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 119 351 N I>3s 15 15 35 351 0.9 0.9 0.7 29.7 5.3 5.3 3.2 22.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.245 1335 Fd-3m 1 1 227 C N N N N 37 2284 0.250 1373 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370018 8.371935 8.362002 90.0285 89.9935 89.9607 ZERR 1.00 0.002030 0.004496 0.000349 0.0149 0.0020 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3693859- 685302 298 263 30 8.8 1037572.49 45.55 0.645 0.601 646864- 460571 232 215 30 7.2 522461.41 30.96 0.832 0.674 454695- 369325 221 211 30 7.0 389316.76 23.92 0.915 0.870 364735- 278324 176 146 30 4.9 217555.88 18.14 0.710 0.660 276439- 197074 193 172 30 5.7 194278.80 18.74 0.710 0.741 190420- 121417 209 184 30 6.1 127339.24 13.97 0.569 0.639 117390- 71463 185 176 30 5.9 90484.16 11.42 0.515 0.473 71046- 50838 103 93 30 3.1 59966.73 9.95 0.344 0.213 50671- 30712 68 60 30 2.0 34610.77 7.35 0.442 0.398 29778- 994 69 67 31 2.2 9075.24 3.39 0.755 0.729 ------------------------------------------------------------------------------------------- 3693859- 994 1754 1587 301 5.3 365565.81 22.51 0.716 0.653 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 330 296 30 9.9 694593.49 41.03 0.699 0.678 0.017 1.08-0.86 335 312 31 10.1 486775.91 25.09 0.840 0.861 0.026 0.83-0.73 248 226 30 7.5 359218.05 20.98 0.663 0.566 0.033 0.72-0.65 209 189 30 6.3 259327.25 17.61 0.698 0.677 0.038 0.65-0.61 160 147 30 4.9 187919.72 13.88 0.854 0.873 0.045 0.60-0.56 151 130 32 4.1 218052.64 15.41 0.435 0.401 0.043 0.56-0.52 135 117 33 3.5 154993.02 14.21 0.570 0.507 0.050 0.52-0.49 101 86 31 2.8 113638.70 11.50 0.495 0.353 0.051 0.49-0.45 56 55 30 1.8 109414.94 12.00 0.443 0.333 0.053 0.45-0.40 29 29 24 1.2 89209.63 11.58 0.362 0.362 0.056 ------------------------------------------------------------------------------------------------------ inf-0.40 1754 1587 301 5.3 365565.81 22.51 0.716 0.653 0.028 inf-0.60 1310 1189 156 7.6 440964.17 25.71 0.735 0.706 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 296 30 30 100.0 9.9 694593.49 142.89 0.699 0.007 1.08-0.86 312 31 31 100.0 10.1 486775.91 94.52 0.840 0.012 0.83-0.73 226 30 30 100.0 7.5 359218.05 70.04 0.663 0.015 0.72-0.65 189 30 30 100.0 6.3 259327.25 52.98 0.698 0.019 0.65-0.61 147 30 30 100.0 4.9 187919.72 40.64 0.854 0.026 0.60-0.56 130 37 32 86.5 4.1 218052.64 35.60 0.435 0.024 0.56-0.52 117 39 33 84.6 3.5 154993.02 32.98 0.570 0.030 0.52-0.49 86 50 31 62.0 2.8 113638.70 23.81 0.495 0.035 0.49-0.45 55 67 30 44.8 1.8 109414.94 18.76 0.443 0.042 0.45-0.40 29 116 24 20.7 1.2 89209.63 13.63 0.362 0.042 -------------------------------------------------------------------------------------------- inf-0.40 1587 460 301 65.4 5.3 365565.81 72.82 0.716 0.016 inf-0.60 1189 156 156 100.0 7.6 440964.17 88.06 0.735 0.013 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 1.0 1.0 -2.0 1.0 1.0 0.0 1.0 No constraint UB - matrix: 0.079517 -0.015538 0.024875 ( 0.000008 0.000007 0.000009 ) 0.029074 0.032861 -0.072544 ( 0.000009 0.000008 0.000010 ) 0.003597 0.076529 0.036247 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.007181 -0.000005 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000005 0.007178 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 0.000004 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: 0.079517 -0.015538 0.024875 ( 0.000008 0.000007 0.000009 ) 0.029074 0.032861 -0.072544 ( 0.000009 0.000008 0.000010 ) 0.003597 0.076529 0.036247 ( 0.000007 0.000006 0.000007 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3701(8) 8.3720(7) 8.3620(9) 90.028(7) 89.994(8) 89.961(7) V = 585.96(10) unit cell: 8.3680(2) 8.3680(2) 8.3680(2) 90.0 90.0 90.0 V = 585.96(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.789) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.789) Run 3 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) PROFFIT INFO: signal sum: min=237.0000 max=20618772.0000 PROFFIT INFO: signal sum lp corr: min=577.5404 max=2944722.9351 PROFFIT INFO: background sum: min=704.0000 max=26070.0000 PROFFIT INFO: background sum sig2: min=525.0000 max=12359.0000 PROFFIT INFO: num of signal pixels: min=49 max=555 PROFFIT INFO: Inet: min=924.0646 max=4711557.0000 PROFFIT INFO: sig(Inet): min=128.1861 max=47452.1914 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.75 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 20 128 326 716 792 1362 2314 3206 3536 Percent 0.0 0.0 0.6 3.6 9.2 20.2 22.4 38.5 65.4 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1768 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1768 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711557- 1234325 176 1945900.41 125.79 100.00 1231453- 740329 176 949150.62 108.75 100.00 739556- 276104 176 476459.53 95.22 100.00 275832- 177543 176 214695.43 74.73 100.00 177369- 135693 176 157893.40 51.76 100.00 134537- 104082 176 117934.44 38.13 100.00 104081- 80032 176 91550.64 30.73 100.00 80018- 6122 176 48098.21 21.34 100.00 6116- 3329 176 4439.96 5.71 98.30 3327- 924 184 2461.16 4.08 66.85 ------------------------------------------------------------------------------------ 4711557- 924 1768 399055.68 55.39 96.38 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 176 731435.25 90.74 100.00 1.39- 1.09 176 814853.82 71.25 100.00 1.09- 0.96 176 373727.74 67.45 97.73 0.96- 0.85 176 413643.37 64.60 95.45 0.85- 0.81 176 495299.06 71.75 99.43 0.81- 0.73 176 264407.54 42.36 99.43 0.73- 0.70 176 194447.06 34.82 85.80 0.70- 0.65 176 356003.19 51.58 97.16 0.65- 0.62 176 184889.23 30.82 90.91 0.62- 0.58 184 172163.78 29.70 97.83 ------------------------------------------------------------------------------------ 4.82- 0.58 1768 399055.68 55.39 96.38 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:28:21 2018 Sorting 1768 observations 84 unique observations with > 7.00 F2/sig(F2) 1768 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 99 307 Total number of frames 307 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1768 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 24 78 Total number of frames 78 1428 observations > 7.00 F2/sig(F2) 1428 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 24 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 15.8 (Out of 1428 removed 5 = 1423, unique = 90) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1423 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 24 78 Total number of frames 78 90 unique data precomputed (should be 90) 90 unique data with 1423 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 15.8 (Out of 1423 removed 0 = 1423, unique = 90) 90 unique data precomputed (should be 90) 90 unique data with 1423 observations RMS deviation of equivalent data = 0.14094 Rint = 0.11555 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11539, wR= 0.14369 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07453, wR= 0.09537, Acormin=0.788, Acormax=1.288, Acor_av=1.011 F test: Probability=1.000, F= 2.388 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07269, wR= 0.08924, Acormin=0.734, Acormax=1.325, Acor_av=0.972 F test: Probability=0.808, F= 1.049 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06055, wR= 0.07728, Acormin=0.707, Acormax=1.328, Acor_av=0.962 F test: Probability=1.000, F= 1.505 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05843, wR= 0.07456, Acormin=0.708, Acormax=1.325, Acor_av=0.913 F test: Probability=0.896, F= 1.072 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04637, wR= 0.06324, Acormin=0.669, Acormax=1.316, Acor_av=0.888 F test: Probability=1.000, F= 1.692 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05740, wR= 0.07368, Acormin=0.715, Acormax=1.316, Acor_av=0.960 F test: Probability=0.000, F= 0.651 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05600, wR= 0.07129, Acormin=0.704, Acormax=1.321, Acor_av=0.906 F test: Probability=0.000, F= 0.682 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04543, wR= 0.06088, Acormin=0.672, Acormax=1.330, Acor_av=0.899 F test: Probability=0.711, F= 1.031 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03627, wR= 0.05120, Acormin=0.525, Acormax=1.187, Acor_av=0.796 F test: Probability=1.000, F= 1.605 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05474, wR= 0.06993, Acormin=0.712, Acormax=1.292, Acor_av=0.932 F test: Probability=0.000, F= 0.440 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05328, wR= 0.06798, Acormin=0.695, Acormax=1.336, Acor_av=0.905 F test: Probability=0.000, F= 0.464 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04007, wR= 0.05526, Acormin=0.531, Acormax=1.077, Acor_av=0.723 F test: Probability=0.000, F= 0.815 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03203, wR= 0.04681, Acormin=0.518, Acormax=1.167, Acor_av=0.776 F test: Probability=1.000, F= 1.265 Trying model 14 (ne=8, no=7)... Results: Rint= 0.02951, wR= 0.04219, Acormin=0.561, Acormax=1.233, Acor_av=0.807 F test: Probability=0.996, F= 1.164 Final absorption model (ne=8, no=7): Rint= 0.02951, Acormin=0.561, Acormax=1.233, Acor_av=0.807 Combined refinement in use Rint: 0.11567 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 157 pars with 12403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14094 Using Levenberg-Marquardt: 0.00010 New wR= 0.03620 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11555 with corrections 0.02626 Rint for all data: 0.11567 with corrections 0.02648 3 observations identified as outliers and rejected Cycle 2 wR= 0.03244 Using Levenberg-Marquardt: 0.00001 New wR= 0.03091 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11514 with corrections 0.02258 Rint for all data: 0.11567 with corrections 0.02639 2 observations identified as outliers and rejected Cycle 3 wR= 0.03021 Using Levenberg-Marquardt: 0.00000 New wR= 0.02992 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11520 with corrections 0.02203 Rint for all data: 0.11567 with corrections 0.02646 0 observations identified as outliers and rejected Cycle 4 wR= 0.02992 Using Levenberg-Marquardt: 0.00000 New wR= 0.02979 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11520 with corrections 0.02199 Rint for all data: 0.11567 with corrections 0.02639 0 observations identified as outliers and rejected Cycle 5 wR= 0.02979 Using Levenberg-Marquardt: 0.00000 New wR= 0.02971 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11520 with corrections 0.02196 Rint for all data: 0.11567 with corrections 0.02633 0 observations identified as outliers and rejected Final wR= 0.02971 Final frame scales: Min= 0.8725 Max= 1.1767 Final absorption correction factors: Amin= 0.5729 Amax= 1.2681 PROFFIT INFO: Inet (after scale3 abspack): min=835.8262 max=6110056.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=131.4549 max=48138.1445 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1768 reflections read from tmp file 131 reflections are rejected (129 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 5 2 5 5 3 2 4 79 Initial Chi^2= 0.28710 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.21084 Current error model SIG(F2)^2 = 112.38*I_RAW + 0.00*I_BACK+(0.00882*)^2 Cycle 2, Chi^2= 1.08294 Current error model SIG(F2)^2 = 63.92*I_RAW + 0.00*I_BACK+(0.01951*)^2 Cycle 3, Chi^2= 1.00528 Current error model SIG(F2)^2 = 86.15*I_RAW + 0.00*I_BACK+(0.01600*)^2 Cycle 4, Chi^2= 1.00013 Current error model SIG(F2)^2 = 82.36*I_RAW + 0.00*I_BACK+(0.01692*)^2 Cycle 5, Chi^2= 1.00007 Current error model SIG(F2)^2 = 83.46*I_RAW + 0.00*I_BACK+(0.01668*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 83.18*I_RAW + 0.00*I_BACK+(0.01675*)^2 Cycle 7, Chi^2= 1.00000 Current error model SIG(F2)^2 = 83.26*I_RAW + 0.00*I_BACK+(0.01673*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 83.26*I_RAW + 0.00*I_BACK+(0.01673*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6110056- 1246580 176 1981317.72 55.17 100.00 1245679- 704461 176 922269.42 47.08 100.00 704022- 298032 176 473157.61 44.65 100.00 297693- 175541 176 217205.14 38.65 100.00 175241- 142947 176 158786.34 31.72 100.00 142016- 99193 176 113742.90 24.56 100.00 99159- 79002 176 89878.31 21.20 100.00 78905- 5820 176 47966.67 15.65 100.00 5789- 3190 176 4258.50 5.77 100.00 3178- 836 184 2479.91 4.78 95.11 ------------------------------------------------------------------------------------ 6110056- 836 1768 399302.51 28.81 99.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 176 779220.38 42.87 100.00 1.39- 1.09 176 828982.04 38.62 100.00 1.09- 0.96 176 374578.47 32.57 100.00 0.96- 0.85 176 414915.61 30.10 100.00 0.85- 0.81 176 484569.36 33.87 100.00 0.81- 0.73 176 257570.21 23.12 100.00 0.73- 0.70 176 187083.05 20.88 96.02 0.70- 0.65 176 340450.44 28.45 100.00 0.65- 0.62 176 174540.12 19.18 98.86 0.62- 0.58 184 161906.18 18.93 100.00 ------------------------------------------------------------------------------------ 4.82- 0.58 1768 399302.51 28.81 99.49 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 176 779220.38 42.87 100.00 4.82- 1.09 352 804101.21 40.75 100.00 4.82- 0.96 528 660926.96 38.02 100.00 4.82- 0.85 704 599424.12 36.04 100.00 4.82- 0.81 880 576453.17 35.61 100.00 4.82- 0.73 1056 523306.01 33.52 100.00 4.82- 0.70 1232 475274.16 31.72 99.43 4.82- 0.65 1408 458421.20 31.31 99.50 4.82- 0.62 1584 426878.85 29.96 99.43 4.82- 0.58 1768 399302.51 28.81 99.49 ------------------------------------------------------------------------------------ 4.82- 0.58 1768 399302.51 28.81 99.49 Scale applied to data: s=0.163664 (maximum obs:6110056.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.026; Rsigma 0.022: data 1768 -> merged 109 With outlier rejection... Rint 0.022; Rsigma 0.023: data 1756 -> merged 109 Rejected total: 12, method kkm 11, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585879, 4.831284 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 9.20 100.00 92 1.61 - 1.21 10 10 16.10 100.00 161 1.17 - 1.01 10 10 20.30 100.00 203 0.99 - 0.89 10 10 20.50 100.00 205 0.88 - 0.81 10 10 19.90 100.00 199 0.81 - 0.74 10 10 16.80 100.00 168 0.73 - 0.71 10 10 19.20 100.00 192 0.70 - 0.66 10 10 16.00 100.00 160 0.66 - 0.64 10 10 14.40 100.00 144 0.63 - 0.60 10 10 14.20 100.00 142 --------------------------------------------------------------- 5.92 - 0.60 100 100 16.66 100.00 1666 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:28:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.915330 5.917811 5.915996 60.0481 90.0549 60.0064 1587 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 773 842 789 801 1202 1061 1067 1587 N (int>3sigma) = 0 608 842 624 628 1037 864 866 1285 Mean intensity = 0.0 50.2 25.6 49.9 56.8 41.5 60.3 58.3 58.8 Mean int/sigma = 0.0 20.8 18.6 20.8 21.6 20.0 23.3 22.8 22.5 Lattice type: P chosen Volume: 146.49 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 5.915 5.915 5.916 90.05 119.98 119.93 Niggli form: a.a = 34.986 b.b = 34.991 c.c = 34.999 b.c = -0.034 a.c = -17.486 a.b = -17.458 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.107 CUBIC F-lattice R(int) = 0.245 [ 1434] Vol = 586.0 Cell: 8.370 8.372 8.362 90.03 89.99 89.96 Volume: 585.95 Matrix:-1.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.088 RHOMBOHEDRAL R-lattice R(int) = 0.188 [ 1171] Vol = 439.5 Cell: 5.921 5.915 14.493 90.02 90.02 120.04 Volume: 439.46 Matrix: 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.088 RHOMBOHEDRAL R-lattice R(int) = 0.183 [ 353] Vol = 439.5 Trigonal Cell: 5.921 5.915 14.493 90.02 90.02 120.04 Volume: 439.46 Matrix: 0.0000 -1.0000 1.0000 1.0000 0.0000 0.0000 -1.0000 2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.025 TETRAGONAL I-lattice R(int) = 0.187 [ 1198] Vol = 293.0 Cell: 5.917 5.921 8.362 89.98 89.98 89.99 Volume: 292.98 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.037 TETRAGONAL I-lattice R(int) = 0.187 [ 1198] Vol = 293.0 Cell: 5.921 5.917 8.362 90.02 90.02 89.99 Volume: 292.98 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.185 [ 1153] Vol = 293.0 Cell: 5.921 5.917 8.362 89.98 89.98 89.99 Volume: 292.98 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.193 [ 1168] Vol = 293.0 Cell: 5.915 8.370 5.918 90.02 89.93 90.03 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.137 [ 939] Vol = 293.0 Cell: 5.917 5.921 8.362 90.02 90.02 89.99 Volume: 292.98 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.043 MONOCLINIC I-lattice R(int) = 0.176 [ 912] Vol = 293.0 Cell: 5.915 5.918 8.370 89.98 90.03 90.07 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.027 MONOCLINIC I-lattice R(int) = 0.146 [ 909] Vol = 293.0 Cell: 5.915 8.370 5.918 90.02 90.07 89.97 Volume: 292.98 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.081 MONOCLINIC C-lattice R(int) = 0.166 [ 941] Vol = 293.0 Cell: 10.252 5.915 5.916 90.05 125.25 89.93 Volume: 292.98 Matrix: 1.0000 -2.0000 2.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.111 [ 579] Vol = 146.5 Cell: 5.915 5.915 5.916 90.05 119.98 119.93 Volume: 146.49 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 842 0 1055 1070 1587 N (int>3sigma) = 0 0 0 0 842 0 858 867 1285 Mean intensity = 0.0 0.0 0.0 0.0 25.6 0.0 59.0 59.0 58.8 Mean int/sigma = 0.0 0.0 0.0 0.0 18.6 0.0 22.5 22.5 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.139 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 119 351 N I>3s 15 15 35 351 0.9 0.9 0.7 29.7 5.3 5.3 3.2 22.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.245 1335 Fd-3m 1 1 227 C N N N N 37 2284 0.250 1373 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370018 8.371935 8.362002 90.0285 89.9935 89.9607 ZERR 1.00 0.002030 0.004496 0.000349 0.0149 0.0020 0.0026 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4834438- 591754 401 396 27 14.7 1335905.41 50.03 0.019 0.022 570916- 135054 512 510 27 18.9 238109.51 37.28 0.027 0.031 119288- 40509 444 444 27 16.4 88618.82 21.05 0.038 0.050 11462- 2004 411 406 28 14.5 3921.00 5.68 0.134 0.166 ------------------------------------------------------------------------------------------- 4834438- 2004 1768 1756 109 16.1 393731.82 28.74 0.022 0.025 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 429 420 27 15.6 693772.31 39.85 0.021 0.022 0.019 1.01-0.78 542 541 28 19.3 381326.11 28.34 0.017 0.022 0.022 0.76-0.65 466 464 27 17.2 287297.54 25.16 0.024 0.029 0.026 0.65-0.59 331 331 27 12.3 182493.10 20.33 0.041 0.043 0.033 ------------------------------------------------------------------------------------------------------ inf-0.59 1768 1756 109 16.1 393731.82 28.74 0.022 0.025 0.023 inf-0.60 1676 1664 99 16.8 408298.65 29.34 0.022 0.025 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 420 27 27 100.0 15.6 693772.31 181.72 0.021 0.008 1.01-0.78 541 28 28 100.0 19.3 381326.11 135.35 0.017 0.005 0.76-0.65 464 27 27 100.0 17.2 287297.54 111.85 0.024 0.007 0.65-0.59 331 28 27 96.4 12.3 182493.10 81.58 0.041 0.011 -------------------------------------------------------------------------------------------- inf-0.59 1756 110 109 99.1 16.1 393731.82 130.09 0.022 0.007 inf-0.60 1664 99 99 100.0 16.8 408298.65 133.58 0.022 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:30:54 2018) ID: 2932; threads 38; handles 877; mem 518620.00 (1229508.00)kB; time: 1w 4d 23h 36m 24s MEMORY INFO: Memory PF:0.0, Ph:220.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:506.5,peak PF: 697.1, WS: 297.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:220.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:508.3,peak PF: 697.1, WS: 299.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:30:54 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000015 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000011 0.000011 ) 5.91502 ( 0.00094 ) 5.91640 ( 0.00095 ) 5.92265 ( 0.00074 ) 60.05206 ( 0.01487 ) 89.98756 ( 0.01148 ) 60.01743 ( 0.01670 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:30:54 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000015 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000011 0.000011 ) M - matrix: 0.021573 -0.014373 0.007199 ( 0.000005 0.000003 0.000003 ) -0.014373 0.028712 -0.014354 ( 0.000003 0.000004 0.000003 ) 0.007199 -0.014354 0.021550 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9150(9) 5.9164(9) 5.9227(7) 60.052(15) 89.988(11) 60.017(17) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.083 ( 0.108) | 1.073 ( 0.135) | 1.145 ( 0.399) | 0.84- 0.81 | 44 | 1.105 ( 0.099) | 1.023 ( 0.124) | 1.367 ( 0.511) | 0.81- 0.73 | 44 | 1.097 ( 0.089) | 0.992 ( 0.126) | 1.341 ( 0.507) | 0.73- 0.69 | 44 | 1.087 ( 0.077) | 0.931 ( 0.109) | 1.374 ( 0.487) | 0.69- 0.66 | 44 | 1.078 ( 0.073) | 0.883 ( 0.089) | 1.403 ( 0.484) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.062 ( 0.110) | 0.998 ( 0.252) | 1.318 ( 0.893) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070035 0.030486 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068374 -0.065763 -0.010701 ( 0.000027 0.000027 0.000015 ) 0.109066 -0.152749 0.115659 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028587 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9266(15) 5.9308(15) 5.9443(11) 60.01(2) 90.017(18) 60.02(3) V = 147.79(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070139 0.030665 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9312(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070139 0.030665 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9296(14) 5.9214(14) 5.9312(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.707) | 1.567 ( 2.299) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.170 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.142) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.029 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.993 ( 0.128) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.383 ( 0.483) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.063 ( 0.108) | 1.003 ( 0.281) | 1.322 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb PROFFITPEAK info: 1381 peaks in the peak location table UB fit with 596 obs out of 641 (total:641,skipped:0) (92.98%) UB - matrix: -0.069842 0.031081 0.088877 ( 0.000053 0.000052 0.000062 ) -0.068944 -0.065591 -0.010256 ( 0.000048 0.000048 0.000056 ) 0.109084 -0.152848 0.116044 ( 0.000064 0.000064 0.000076 ) M - matrix: 0.021531 -0.014322 0.007158 ( 0.000017 0.000013 0.000013 ) -0.014322 0.028631 -0.014302 ( 0.000013 0.000021 0.000015 ) 0.007158 -0.014302 0.021471 ( 0.000013 0.000015 0.000021 ) unit cell: 5.918(3) 5.924(3) 5.926(3) 60.03(5) 90.02(4) 60.03(5) V = 147.01(12) UB fit with 596 obs out of 641 (total:641,skipped:0) (92.98%) UB - matrix: -0.069842 0.031081 0.088877 ( 0.000053 0.000052 0.000062 ) -0.068944 -0.065591 -0.010256 ( 0.000048 0.000048 0.000056 ) 0.109084 -0.152848 0.116044 ( 0.000064 0.000064 0.000076 ) M - matrix: 0.021531 -0.014322 0.007158 ( 0.000017 0.000013 0.000013 ) -0.014322 0.028631 -0.014302 ( 0.000013 0.000021 0.000015 ) 0.007158 -0.014302 0.021471 ( 0.000013 0.000015 0.000021 ) unit cell: 5.918(3) 5.924(3) 5.926(3) 60.03(5) 90.02(4) 60.03(5) V = 147.01(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069870 0.031108 0.088779 ( 0.000051 0.000051 0.000060 ) -0.068869 -0.065693 -0.010272 ( 0.000050 0.000050 0.000059 ) 0.108989 -0.152690 0.116068 ( 0.000063 0.000063 0.000074 ) M - matrix: 0.021503 -0.014291 0.007155 ( 0.000017 0.000013 0.000013 ) -0.014291 0.028597 -0.014286 ( 0.000013 0.000020 0.000015 ) 0.007155 -0.014286 0.021459 ( 0.000013 0.000015 0.000020 ) UB fit with 600 obs out of 641 (total:641,skipped:0) (93.60%) unit cell: 5.919(3) 5.923(3) 5.927(3) 60.05(5) 90.06(4) 60.08(5) V = 147.13(12) UB fit with 600 obs out of 641 (total:641,skipped:0) (93.60%) UB - matrix: -0.069870 0.031108 0.088779 ( 0.000051 0.000051 0.000060 ) -0.068869 -0.065693 -0.010272 ( 0.000050 0.000050 0.000059 ) 0.108989 -0.152690 0.116068 ( 0.000063 0.000063 0.000074 ) M - matrix: 0.021503 -0.014291 0.007155 ( 0.000017 0.000013 0.000013 ) -0.014291 0.028597 -0.014286 ( 0.000013 0.000020 0.000015 ) 0.007155 -0.014286 0.021459 ( 0.000013 0.000015 0.000020 ) unit cell: 5.919(3) 5.923(3) 5.927(3) 60.05(5) 90.06(4) 60.08(5) V = 147.13(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 641 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=53.000) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069870 0.031108 0.088779 ( 0.000051 0.000051 0.000060 ) -0.068869 -0.065693 -0.010272 ( 0.000050 0.000050 0.000059 ) 0.108989 -0.152690 0.116068 ( 0.000063 0.000063 0.000074 ) M - matrix: 0.021503 -0.014291 0.007155 ( 0.000017 0.000013 0.000013 ) -0.014291 0.028597 -0.014286 ( 0.000013 0.000020 0.000015 ) 0.007155 -0.014286 0.021459 ( 0.000013 0.000015 0.000020 ) UB fit with 600 obs out of 641 (total:641,skipped:0) (93.60%) unit cell: 5.919(3) 5.923(3) 5.927(3) 60.05(5) 90.06(4) 60.08(5) V = 147.13(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 601 obs out of 641 (total:641,skipped:0) (93.76%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 6 of 483 peaks identified as outliers and rejected 477 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 477 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 477 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.41 | 48 | 1.011 ( 0.158) | 1.177 ( 0.600) | 1.154 ( 0.716) | 1.41- 1.17 | 48 | 1.040 ( 0.122) | 1.173 ( 0.470) | 0.975 ( 0.500) | 1.17- 1.01 | 48 | 0.993 ( 0.091) | 1.040 ( 0.259) | 1.003 ( 0.447) | 0.99- 0.92 | 48 | 1.026 ( 0.073) | 1.024 ( 0.096) | 1.108 ( 0.432) | 0.92- 0.82 | 48 | 0.999 ( 0.078) | 0.985 ( 0.116) | 1.122 ( 0.406) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.960 ( 0.111) | 1.083 ( 0.434) | 0.75- 0.71 | 48 | 0.978 ( 0.042) | 0.909 ( 0.059) | 1.250 ( 0.522) | 0.71- 0.66 | 48 | 0.950 ( 0.049) | 0.858 ( 0.052) | 1.226 ( 0.479) | 0.66- 0.62 | 48 | 0.926 ( 0.045) | 0.839 ( 0.039) | 1.167 ( 0.424) | 0.62- 0.59 | 45 | 0.904 ( 0.043) | 0.813 ( 0.039) | 1.329 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 477 | 0.983 ( 0.095) | 0.979 ( 0.291) | 1.141 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 477 obs out of 477 (total:477,skipped:0) (100.00%) UB - matrix: -0.069970 0.031027 0.088990 ( 0.000028 0.000026 0.000030 ) -0.068567 -0.066039 -0.010152 ( 0.000022 0.000020 0.000024 ) 0.108965 -0.152897 0.116303 ( 0.000022 0.000020 0.000023 ) M - matrix: 0.021470 -0.014303 0.007142 ( 0.000007 0.000005 0.000005 ) -0.014303 0.028701 -0.014351 ( 0.000005 0.000007 0.000005 ) 0.007142 -0.014351 0.021549 ( 0.000005 0.000005 0.000008 ) unit cell: 5.9227(13) 5.9163(13) 5.9163(14) 59.98(2) 89.963(19) 60.05(2) V = 146.71(5) OTKP changes: 477 1 1 1 UB - matrix: -0.069858 0.030985 0.088977 ( 0.000025 0.000024 0.000028 ) -0.068803 -0.065803 -0.010207 ( 0.000018 0.000017 0.000020 ) 0.109159 -0.152975 0.116322 ( 0.000021 0.000020 0.000023 ) M - matrix: 0.021530 -0.014336 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014336 0.028691 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014366 0.021552 ( 0.000005 0.000005 0.000007 ) UB fit with 477 obs out of 477 (total:477,skipped:0) (100.00%) unit cell: 5.9177(12) 5.9206(11) 5.9193(13) 59.98(2) 90.025(17) 60.05(2) V = 146.68(5) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.904) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069858 0.030985 0.088977 ( 0.000025 0.000024 0.000028 ) -0.068803 -0.065803 -0.010207 ( 0.000018 0.000017 0.000020 ) 0.109159 -0.152975 0.116322 ( 0.000021 0.000020 0.000023 ) M - matrix: 0.021530 -0.014336 0.007184 ( 0.000006 0.000005 0.000005 ) -0.014336 0.028691 -0.014366 ( 0.000005 0.000007 0.000005 ) 0.007184 -0.014366 0.021552 ( 0.000005 0.000005 0.000007 ) UB fit with 477 obs out of 477 (total:477,skipped:0) (100.00%) unit cell: 5.9177(12) 5.9206(11) 5.9193(13) 59.98(2) 90.025(17) 60.05(2) V = 146.68(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 477 obs out of 477 (total:477,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 488 peaks identified as outliers and rejected 480 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 480 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 480 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.4 | 133 | 1.119 ( 0.120) | 1.252 ( 0.457) | 1.225 ( 1.367) | 13.5-19.2 | 133 | 1.078 ( 0.056) | 1.127 ( 0.245) | 1.202 ( 0.531) | 19.2-23.3 | 133 | 1.074 ( 0.079) | 1.148 ( 0.379) | 1.168 ( 0.492) | 23.4-27.3 | 133 | 1.033 ( 0.085) | 1.083 ( 0.322) | 1.229 ( 0.593) | 27.3-30.9 | 133 | 1.015 ( 0.080) | 1.006 ( 0.186) | 1.239 ( 0.507) | 31.0-33.9 | 133 | 0.980 ( 0.091) | 0.923 ( 0.101) | 1.183 ( 0.511) | 33.9-37.0 | 134 | 0.968 ( 0.082) | 0.894 ( 0.093) | 1.210 ( 0.510) | 37.0-39.8 | 133 | 0.948 ( 0.098) | 0.883 ( 0.158) | 1.164 ( 0.553) | 39.9-42.9 | 134 | 0.928 ( 0.090) | 0.840 ( 0.088) | 1.180 ( 0.514) | 42.9-49.9 | 128 | 0.936 ( 0.087) | 0.817 ( 0.069) | 1.171 ( 0.453) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1327 | 1.008 ( 0.108) | 0.998 ( 0.284) | 1.197 ( 0.657) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0098 b=1.26 e3 dimension: a=0.0029 b=0.97 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706999 Maximum peak integral for reflections I/sig<= 10000 - raw: 23928508 lp-corr: 2786922 PROFFITPEAK - Finished at Tue Mar 27 14:31:12 2018 PROFFITMAIN - Started at Tue Mar 27 14:31:12 2018 OTKP changes: 1327 2 3 3 OTKP changes: 1327 2 3 3 UB - matrix: -0.070204 0.031078 0.088927 ( 0.000016 0.000014 0.000013 ) -0.068776 -0.065844 -0.010525 ( 0.000016 0.000014 0.000013 ) 0.109225 -0.153077 0.116348 ( 0.000014 0.000012 0.000011 ) M - matrix: 0.021589 -0.014373 0.007189 ( 0.000004 0.000003 0.000003 ) -0.014373 0.028734 -0.014353 ( 0.000003 0.000004 0.000003 ) 0.007189 -0.014353 0.021555 ( 0.000003 0.000003 0.000004 ) UB fit with 1327 obs out of 1327 (total:1327,skipped:0) (100.00%) unit cell: 5.9110(9) 5.9133(9) 5.9138(7) 60.049(14) 90.037(11) 60.020(15) V = 146.27(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070061 0.030673 0.088950 ( 0.000028 0.000028 0.000016 ) -0.068233 -0.066136 -0.010524 ( 0.000025 0.000025 0.000014 ) 0.109080 -0.153066 0.115993 ( 0.000025 0.000024 0.000014 ) M - matrix: 0.021463 -0.014333 0.007139 ( 0.000008 0.000006 0.000004 ) -0.014333 0.028744 -0.014330 ( 0.000006 0.000008 0.000004 ) 0.007139 -0.014330 0.021477 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9281(14) 5.9138(14) 5.9247(11) 60.02(2) 89.973(18) 60.00(2) V = 146.94(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070343 0.030952 0.088806 ( 0.000026 0.000026 0.000015 ) -0.068416 -0.066141 -0.010677 ( 0.000024 0.000023 0.000013 ) 0.109344 -0.153297 0.116383 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014414 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014414 0.028833 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014386 0.021546 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9152(13) 5.9069(13) 5.9175(10) 60.05(2) 90.069(16) 60.00(2) V = 146.22(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.783) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070343 0.030952 0.088806 ( 0.000026 0.000026 0.000015 ) -0.068416 -0.066141 -0.010677 ( 0.000024 0.000023 0.000013 ) 0.109344 -0.153297 0.116383 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014414 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014414 0.028833 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014386 0.021546 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9152(13) 5.9069(13) 5.9175(10) 60.05(2) 90.069(16) 60.00(2) V = 146.22(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070343 0.030952 0.088806 ( 0.000026 0.000026 0.000015 ) -0.068416 -0.066141 -0.010677 ( 0.000024 0.000023 0.000013 ) 0.109344 -0.153297 0.116383 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014414 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014414 0.028833 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014386 0.021546 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9152(13) 5.9069(13) 5.9175(10) 60.05(2) 90.069(16) 60.00(2) V = 146.22(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031340 0.088628 ( 0.000025 0.000022 0.000027 ) -0.068586 -0.065989 -0.010251 ( 0.000031 0.000027 0.000033 ) 0.108997 -0.152673 0.116253 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021542 -0.014322 0.007134 ( 0.000007 0.000005 0.000005 ) -0.014322 0.028646 -0.014295 ( 0.000005 0.000006 0.000005 ) 0.007134 -0.014295 0.021475 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9146(16) 5.9210(16) 5.9229(13) 60.03(3) 89.95(2) 60.01(3) V = 146.81(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070364 0.031215 0.088852 ( 0.000023 0.000020 0.000025 ) -0.068804 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153168 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014387 0.007189 ( 0.000007 0.000005 0.000005 ) -0.014387 0.028771 -0.014403 ( 0.000005 0.000006 0.000005 ) 0.007189 -0.014403 0.021596 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9089(16) 5.9158(16) 5.9138(12) 59.94(2) 89.948(19) 60.01(3) V = 146.12(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.783) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070364 0.031215 0.088852 ( 0.000023 0.000020 0.000025 ) -0.068804 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153168 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014387 0.007189 ( 0.000007 0.000005 0.000005 ) -0.014387 0.028771 -0.014403 ( 0.000005 0.000006 0.000005 ) 0.007189 -0.014403 0.021596 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9089(16) 5.9158(16) 5.9138(12) 59.94(2) 89.948(19) 60.01(3) V = 146.12(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070364 0.031215 0.088852 ( 0.000023 0.000020 0.000025 ) -0.068804 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153168 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014387 0.007189 ( 0.000007 0.000005 0.000005 ) -0.014387 0.028771 -0.014403 ( 0.000005 0.000006 0.000005 ) 0.007189 -0.014403 0.021596 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9089(16) 5.9158(16) 5.9138(12) 59.94(2) 89.948(19) 60.01(3) V = 146.12(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 480 (total:480,skipped:0) (100.00%) UB - matrix: -0.069963 0.030980 0.089005 ( 0.000027 0.000025 0.000030 ) -0.068699 -0.065988 -0.010227 ( 0.000019 0.000017 0.000020 ) 0.109072 -0.152949 0.116344 ( 0.000023 0.000021 0.000025 ) M - matrix: 0.021511 -0.014317 0.007165 ( 0.000007 0.000005 0.000005 ) -0.014317 0.028707 -0.014362 ( 0.000005 0.000007 0.000005 ) 0.007165 -0.014362 0.021562 ( 0.000005 0.000005 0.000008 ) unit cell: 5.9167(12) 5.9150(12) 5.9156(14) 59.98(2) 90.011(18) 60.08(2) V = 146.53(5) OTKP changes: 480 1 1 1 UB - matrix: -0.069859 0.030984 0.088977 ( 0.000027 0.000025 0.000029 ) -0.068769 -0.065839 -0.010199 ( 0.000017 0.000016 0.000018 ) 0.109139 -0.152953 0.116334 ( 0.000023 0.000021 0.000025 ) M - matrix: 0.021521 -0.014330 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014330 0.028689 -0.014365 ( 0.000005 0.000007 0.000005 ) 0.007182 -0.014365 0.021554 ( 0.000005 0.000005 0.000008 ) UB fit with 480 obs out of 480 (total:480,skipped:0) (100.00%) unit cell: 5.9184(11) 5.9203(11) 5.9187(13) 59.98(2) 90.028(17) 60.06(2) V = 146.69(5) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) HKL list info: 788 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069859 0.030984 0.088977 ( 0.000027 0.000025 0.000029 ) -0.068769 -0.065839 -0.010199 ( 0.000017 0.000016 0.000018 ) 0.109139 -0.152953 0.116334 ( 0.000023 0.000021 0.000025 ) M - matrix: 0.021521 -0.014330 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014330 0.028689 -0.014365 ( 0.000005 0.000007 0.000005 ) 0.007182 -0.014365 0.021554 ( 0.000005 0.000005 0.000008 ) UB fit with 480 obs out of 480 (total:480,skipped:0) (100.00%) unit cell: 5.9184(11) 5.9203(11) 5.9187(13) 59.98(2) 90.028(17) 60.06(2) V = 146.69(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 480 (total:480,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* UB - matrix: -0.069859 0.030984 0.088977 ( 0.000027 0.000025 0.000029 ) -0.068769 -0.065839 -0.010199 ( 0.000017 0.000016 0.000018 ) 0.109139 -0.152953 0.116334 ( 0.000023 0.000021 0.000025 ) M - matrix: 0.021521 -0.014330 0.007182 ( 0.000007 0.000005 0.000005 ) -0.014330 0.028689 -0.014365 ( 0.000005 0.000007 0.000005 ) 0.007182 -0.014365 0.021554 ( 0.000005 0.000005 0.000008 ) UB fit with 480 obs out of 480 (total:480,skipped:0) (100.00%) unit cell: 5.9184(11) 5.9203(11) 5.9187(13) 59.98(2) 90.028(17) 60.06(2) V = 146.69(5) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070171 0.031078 0.088854 ( 0.000017 0.000014 0.000014 ) -0.068769 -0.065737 -0.010584 ( 0.000019 0.000016 0.000015 ) 0.109177 -0.153056 0.116379 ( 0.000014 0.000012 0.000011 ) M - matrix: 0.021573 -0.014370 0.007199 ( 0.000005 0.000003 0.000003 ) -0.014370 0.028713 -0.014355 ( 0.000003 0.000004 0.000003 ) 0.007199 -0.014355 0.021551 ( 0.000003 0.000003 0.000004 ) UB fit with 1327 obs out of 1327 (total:1327,skipped:0) (100.00%) unit cell: 5.9148(9) 5.9174(9) 5.9161(7) 60.043(15) 90.057(11) 60.016(17) V = 146.48(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 60 reflections under beam stop or inside a detector rejection region 13 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof 1812 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:31:17 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.783) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.783) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2944967.9642 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4711949.0000 PROFFIT INFO: sig(Inet): min=128.9277 max=47455.9336 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.62 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 10 66 169 368 407 700 1187 1644 1812 Percent 0.0 0.0 0.6 3.6 9.3 20.3 22.5 38.6 65.5 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1812 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1812 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711949- 1230600 181 1937979.52 125.98 100.00 1228602- 726371 181 938826.66 107.61 100.00 720025- 272491 181 464187.53 95.92 100.00 272200- 178077 181 212740.61 73.93 100.00 178050- 133212 181 157490.06 51.61 100.00 133179- 103330 181 116958.64 37.71 100.00 103180- 78480 181 90350.28 30.52 100.00 78362- 5968 181 45424.49 20.57 100.00 5951- 3234 181 4323.89 5.64 97.79 3230- 924 183 2431.66 4.06 66.12 ------------------------------------------------------------------------------------ 4711949- 924 1812 396635.75 55.30 96.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 181 709807.91 87.70 98.90 1.32- 1.05 181 581935.16 67.87 97.79 1.05- 0.92 181 495951.74 64.89 97.79 0.92- 0.82 181 354964.31 54.54 95.58 0.82- 0.74 181 420339.97 58.59 96.69 0.74- 0.67 181 386053.58 55.24 96.13 0.67- 0.62 181 267361.89 44.77 96.69 0.62- 0.57 181 322558.72 48.16 92.82 0.57- 0.52 181 226822.04 38.24 96.69 0.52- 0.40 183 202705.06 33.24 94.54 ------------------------------------------------------------------------------------ 5.26- 0.40 1812 396635.75 55.30 96.36 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:31:17 2018 Sorting 1812 observations 235 unique observations with > 7.00 F2/sig(F2) 1812 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 Total number of frames 314 Maximum number of 235 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1812 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 Total number of frames 159 1463 observations > 7.00 F2/sig(F2) 1463 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 Total number of frames 159 Removing 'redundancy=1' reflections Average redundancy: 6.2 (Out of 1463 removed 50 = 1413, unique = 229) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1413 observations in 3 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 Total number of frames 159 229 unique data precomputed (should be 229) 229 unique data with 1413 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.2 (Out of 1413 removed 0 = 1413, unique = 229) 229 unique data precomputed (should be 229) 229 unique data with 1413 observations RMS deviation of equivalent data = 0.70107 Rint = 0.67013 11 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.64326, wR= 3.68992 Trying model 1 (ne=2, no=0)... Results: Rint= 0.71742, wR= 2.66784, Acormin=-0.001, Acormax=2.093, Acor_av=0.625 F test: Probability=0.000, F= 0.801 Trying model 2 (ne=2, no=1)... Results: Rint= 0.88989, wR= 2.70380, Acormin=-0.354, Acormax=1.877, Acor_av=0.357 F test: Probability=0.000, F= 0.519 Trying model 3 (ne=4, no=0)... Results: Rint= 0.74597, wR= 2.16048, Acormin=-0.117, Acormax=2.189, Acor_av=0.500 F test: Probability=0.000, F= 0.735 Trying model 4 (ne=4, no=1)... Results: Rint= 0.88842, wR= 2.31119, Acormin=-0.516, Acormax=1.996, Acor_av=0.284 F test: Probability=0.000, F= 0.517 Trying model 5 (ne=4, no=3)... Results: Rint= 0.96665, wR= 2.08247, Acormin=-1.102, Acormax=1.464, Acor_av=0.080 F test: Probability=0.000, F= 0.434 Trying model 6 (ne=6, no=0)... Results: Rint= 0.78719, wR= 2.26480, Acormin=-0.218, Acormax=2.783, Acor_av=0.427 F test: Probability=0.000, F= 0.652 Trying model 7 (ne=6, no=1)... Results: Rint= 0.91650, wR= 2.47645, Acormin=-0.600, Acormax=2.259, Acor_av=0.210 F test: Probability=0.000, F= 0.480 Trying model 8 (ne=6, no=3)... Results: Rint= 0.97000, wR= 2.43204, Acormin=-1.157, Acormax=1.493, Acor_av=0.066 F test: Probability=0.000, F= 0.426 Trying model 9 (ne=6, no=5)... Results: Rint= 1.02058, wR= 2.16976, Acormin=-0.507, Acormax=1.901, Acor_av=0.010 F test: Probability=0.000, F= 0.381 Trying model 10 (ne=8, no=0)... Results: Rint= 0.85258, wR= 1.87840, Acormin=-0.598, Acormax=3.250, Acor_av=0.322 F test: Probability=0.000, F= 0.548 Trying model 11 (ne=8, no=1)... Results: Rint= 1.01987, wR= 2.03212, Acormin=-1.021, Acormax=1.364, Acor_av=0.030 F test: Probability=0.000, F= 0.382 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98005, wR= 1.35592, Acormin=-0.043, Acormax=0.081, Acor_av=0.002 F test: Probability=0.000, F= 0.411 Trying model 13 (ne=8, no=5)... Results: Rint= 0.97861, wR= 1.36429, Acormin=-0.042, Acormax=0.083, Acor_av=0.002 F test: Probability=0.000, F= 0.408 Trying model 14 (ne=8, no=7)... Results: Rint= 0.98871, wR= 1.47631, Acormin=-0.052, Acormax=0.079, Acor_av=0.000 F test: Probability=0.000, F= 0.394 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.83629 There are 159 active scales (one needs to be fixed) Refinement control: frame scale #137 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.70107 Using Levenberg-Marquardt: 0.00010 New wR= 0.68175 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67013 with corrections 0.64609 Rint for all data: 0.83629 with corrections 0.81797 11 observations identified as outliers and rejected Cycle 2 wR= 0.64276 Using Levenberg-Marquardt: 0.00001 New wR= 0.63921 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64326 with corrections 0.61925 Rint for all data: 0.83629 with corrections 0.81972 6 observations identified as outliers and rejected Cycle 3 wR= 0.61689 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61251 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63426 with corrections 0.61265 Rint for all data: 0.83629 with corrections 0.82207 6 observations identified as outliers and rejected Cycle 4 wR= 0.60546 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.60698 Using Levenberg-Marquardt: 0.10000 New wR= 0.60411 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63128 with corrections 0.61232 Rint for all data: 0.83629 with corrections 0.82314 5 observations identified as outliers and rejected Cycle 5 wR= 0.59445 Using Levenberg-Marquardt: 0.01000 New wR= 0.59652 Using Levenberg-Marquardt: 0.10000 New wR= 0.59296 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.62897 with corrections 0.61185 Rint for all data: 0.83629 with corrections 0.82459 3 observations identified as outliers and rejected Final wR= 0.59296 Final frame scales: Min= 0.8889 Max= 2.9529 Final absorption correction factors: Amin= 0.4462 Amax= 1.5349 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=703.7510 max=5744154.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=127.7823 max=69489.2656 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/3 frame:1/108 1811 reflections read from tmp file 1381 reflections are rejected (1286 as outliers, 95 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 75 39 14 14 1 2 1 1 Initial Chi^2= 0.69174 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94085 Current error model SIG(F2)^2 = 321.25*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 302.24*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 302.24*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5744154- 1221510 181 1982424.31 84.81 100.00 1218707- 630152 181 894543.65 42.76 100.00 621026- 276704 181 421774.92 38.59 100.00 276309- 178848 181 220320.08 28.05 100.00 177568- 134091 181 153424.44 19.11 100.00 134091- 98291 181 117442.31 15.82 100.00 98237- 66359 181 81519.41 12.11 100.00 66256- 5930 181 38701.69 8.87 90.61 5915- 2998 181 4062.86 3.03 28.18 2985- 704 182 2233.23 2.48 14.29 ------------------------------------------------------------------------------------ 5744154- 704 1811 391429.66 25.55 83.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 181 833677.31 55.31 95.58 1.32- 1.05 181 582644.02 37.75 91.16 1.05- 0.92 181 536167.47 30.33 88.40 0.92- 0.82 181 350477.71 22.84 78.45 0.82- 0.74 181 413053.27 24.31 86.74 0.74- 0.67 181 352334.21 21.59 77.35 0.67- 0.62 181 239143.07 17.25 80.11 0.62- 0.57 181 284246.65 18.40 81.22 0.57- 0.52 181 185541.38 14.96 80.11 0.52- 0.40 182 138409.46 12.83 73.63 ------------------------------------------------------------------------------------ 5.26- 0.40 1811 391429.66 25.55 83.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 181 833677.31 55.31 95.58 5.26- 1.05 362 708160.66 46.53 93.37 5.26- 0.92 543 650829.60 41.13 91.71 5.26- 0.82 724 575741.63 36.56 88.40 5.26- 0.74 905 543203.95 34.11 88.07 5.26- 0.67 1086 511392.33 32.02 86.28 5.26- 0.62 1267 472499.58 29.91 85.40 5.26- 0.57 1448 448967.96 28.47 84.88 5.26- 0.52 1629 419698.34 26.97 84.35 5.26- 0.40 1811 391429.66 25.55 83.27 ------------------------------------------------------------------------------------ 5.26- 0.40 1811 391429.66 25.55 83.27 Scale applied to data: s=0.174090 (maximum obs:5744154.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.824; Rsigma 0.025: data 1811 -> merged 302 With outlier rejection... Rint 0.716; Rsigma 0.027: data 1666 -> merged 302 Rejected total: 145, method kkm 134, method Blessing 11 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404295, 5.271356 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 8.00 100.00 120 1.46 - 1.12 15 15 12.33 100.00 185 1.08 - 0.96 15 15 10.87 100.00 163 0.96 - 0.86 15 15 10.13 100.00 152 0.86 - 0.79 15 15 8.53 100.00 128 0.79 - 0.73 15 15 7.93 100.00 119 0.73 - 0.69 15 15 6.53 100.00 98 0.69 - 0.65 15 15 6.80 100.00 102 0.65 - 0.63 15 15 4.33 100.00 65 0.63 - 0.60 21 21 5.05 100.00 106 --------------------------------------------------------------- 5.92 - 0.60 156 156 7.94 100.00 1238 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:31:17 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914808 5.917426 5.916140 60.0430 90.0569 60.0158 1666 Reflections read from file xs1714a.hkl; mean (I/sigma) = 24.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 819 887 826 840 1266 1120 1127 1666 N (int>3sigma) = 0 668 887 675 679 1115 937 932 1380 Mean intensity = 0.0 53.1 27.3 52.9 60.9 44.0 63.8 62.3 61.8 Mean int/sigma = 0.0 22.6 20.7 22.6 23.9 22.0 25.3 25.0 24.5 Lattice type: P chosen Volume: 146.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Unitcell: 5.915 5.915 5.916 119.98 90.06 119.94 Niggli form: a.a = 34.985 b.b = 34.986 c.c = 35.001 b.c = -17.485 a.c = -0.035 a.b = -17.458 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.083 CUBIC F-lattice R(int) = 0.194 [ 1512] Vol = 585.9 Cell: 8.362 8.372 8.370 89.97 89.99 90.02 Volume: 585.90 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 1244] Vol = 439.4 Cell: 5.915 5.915 14.494 89.98 90.04 119.94 Volume: 439.43 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 373] Vol = 439.4 Trigonal Cell: 5.915 5.915 14.494 89.98 90.04 119.94 Volume: 439.43 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.052 TETRAGONAL I-lattice R(int) = 0.152 [ 1275] Vol = 293.0 Cell: 5.921 5.918 8.362 89.97 90.01 90.01 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.039 TETRAGONAL I-lattice R(int) = 0.152 [ 1275] Vol = 293.0 Cell: 5.921 5.918 8.362 89.97 90.01 90.01 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.154 [ 1228] Vol = 293.0 Cell: 5.921 8.362 5.918 89.97 89.99 89.99 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.126 [ 1013] Vol = 293.0 Cell: 8.362 5.921 5.918 90.01 90.03 89.99 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC C-lattice R(int) = 0.139 [ 1024] Vol = 293.0 Cell: 8.362 8.372 5.915 89.96 134.97 90.02 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.104 [ 621] Vol = 146.5 Cell: 5.915 5.915 5.916 119.98 90.06 119.94 Volume: 146.48 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 887 0 1120 1127 1666 N (int>3sigma) = 0 0 0 0 887 0 937 934 1380 Mean intensity = 0.0 0.0 0.0 0.0 27.3 0.0 63.8 61.5 61.8 Mean int/sigma = 0.0 0.0 0.0 0.0 20.7 0.0 25.3 24.3 24.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.109 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 23 23 129 375 N I>3s 20 20 55 375 0.9 0.9 0.7 31.4 5.7 5.7 3.5 25.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.194 1403 Fd-3m 1 1 227 C N N N N 37 2284 0.197 1441 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361589 8.371788 8.369897 89.9700 89.9871 90.0248 ZERR 1.00 0.000354 0.004494 0.002020 0.0027 0.0020 0.0148 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3379295- 698089 267 235 30 7.8 1048999.55 51.44 0.611 0.566 686859- 511847 238 223 30 7.4 526897.00 35.28 0.811 0.675 509091- 380628 218 213 30 7.1 433328.70 28.77 0.952 0.927 379080- 288980 208 182 30 6.1 251001.32 19.31 0.818 0.775 287208- 202122 197 164 30 5.5 177351.77 18.63 0.730 0.770 198528- 117216 246 230 30 7.7 139023.99 16.82 0.565 0.652 115789- 81897 169 159 30 5.3 97979.38 12.95 0.505 0.432 81033- 57676 102 98 30 3.3 73679.49 11.48 0.301 0.221 57565- 37566 94 91 30 3.0 48671.77 8.57 0.666 0.564 37161- 1294 72 71 32 2.2 12742.59 3.88 0.772 0.743 ------------------------------------------------------------------------------------------- 3379295- 1294 1811 1666 302 5.5 354855.07 24.47 0.716 0.662 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 338 305 30 10.2 629901.66 45.55 0.701 0.707 0.016 1.08-0.86 345 325 31 10.5 472096.85 27.59 0.836 0.864 0.024 0.83-0.73 258 240 30 8.0 352015.69 22.30 0.684 0.594 0.030 0.72-0.65 227 201 32 6.3 242567.59 18.04 0.664 0.624 0.036 0.65-0.60 169 153 30 5.1 236041.87 16.36 0.750 0.770 0.037 0.60-0.56 157 148 32 4.6 206924.66 15.77 0.533 0.480 0.042 0.56-0.52 127 114 31 3.7 186610.69 15.63 0.646 0.614 0.044 0.52-0.49 99 92 30 3.1 128290.61 11.93 0.592 0.437 0.050 0.49-0.45 60 57 30 1.9 160650.67 14.42 0.319 0.249 0.044 0.45-0.40 31 31 26 1.2 110468.45 12.37 0.396 0.396 0.052 ------------------------------------------------------------------------------------------------------ inf-0.40 1811 1666 302 5.5 354855.07 24.47 0.716 0.662 0.027 inf-0.60 1352 1238 156 7.9 420531.47 28.04 0.737 0.720 0.024 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 305 30 30 100.0 10.2 629901.66 160.95 0.701 0.006 1.08-0.86 325 31 31 100.0 10.5 472096.85 106.98 0.836 0.011 0.83-0.73 240 30 30 100.0 8.0 352015.69 77.66 0.684 0.014 0.72-0.65 201 32 32 100.0 6.3 242567.59 54.25 0.664 0.018 0.65-0.60 153 30 30 100.0 5.1 236041.87 48.96 0.750 0.022 0.60-0.56 148 37 32 86.5 4.6 206924.66 40.03 0.533 0.021 0.56-0.52 114 36 31 86.1 3.7 186610.69 37.91 0.646 0.027 0.52-0.49 92 47 30 63.8 3.1 128290.61 26.25 0.592 0.033 0.49-0.45 57 64 30 46.9 1.9 160650.67 22.98 0.319 0.034 0.45-0.40 31 126 26 20.6 1.2 110468.45 14.48 0.396 0.038 -------------------------------------------------------------------------------------------- inf-0.40 1666 464 302 65.1 5.5 354855.07 81.22 0.716 0.015 inf-0.60 1238 156 156 100.0 7.9 420531.47 98.38 0.737 0.012 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 -1.0 No constraint UB - matrix: -0.024880 0.015539 -0.079512 ( 0.000009 0.000007 0.000008 ) 0.072545 -0.032868 -0.029092 ( 0.000010 0.000008 0.000009 ) -0.036250 -0.076527 -0.003601 ( 0.000008 0.000006 0.000007 ) M - matrix: 0.007196 0.000003 -0.000002 ( 0.000002 0.000001 0.000001 ) 0.000003 0.007178 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000004 0.007182 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024880 0.015539 -0.079512 ( 0.000009 0.000007 0.000008 ) 0.072545 -0.032868 -0.029092 ( 0.000010 0.000008 0.000009 ) -0.036250 -0.076527 -0.003601 ( 0.000008 0.000006 0.000007 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3616(9) 8.3719(7) 8.3699(8) 89.970(7) 89.987(8) 90.025(7) V = 585.91(10) unit cell: 8.3678(2) 8.3678(2) 8.3678(2) 90.0 90.0 90.0 V = 585.91(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.783) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.783) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2944967.9642 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4711949.0000 PROFFIT INFO: sig(Inet): min=128.9277 max=47455.9336 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.62 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 20 132 338 736 814 1400 2374 3288 3624 Percent 0.0 0.0 0.6 3.6 9.3 20.3 22.5 38.6 65.5 90.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1812 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1812 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711949- 1230600 181 1937979.52 125.98 100.00 1228602- 726371 181 938826.66 107.61 100.00 720025- 272491 181 464187.53 95.92 100.00 272200- 178077 181 212740.61 73.93 100.00 178050- 133212 181 157490.06 51.61 100.00 133179- 103330 181 116958.64 37.71 100.00 103180- 78480 181 90350.28 30.52 100.00 78362- 5968 181 45424.49 20.57 100.00 5951- 3234 181 4323.89 5.64 97.79 3230- 924 183 2431.66 4.06 66.12 ------------------------------------------------------------------------------------ 4711949- 924 1812 396635.75 55.30 96.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 181 720519.22 91.39 100.00 1.39- 1.09 181 810966.62 70.98 100.00 1.09- 0.96 181 377480.09 67.72 97.79 0.96- 0.85 181 412245.82 64.52 95.58 0.85- 0.81 181 482882.40 70.36 99.45 0.81- 0.73 181 263426.62 42.14 99.45 0.73- 0.70 181 206713.66 36.09 86.19 0.70- 0.65 181 337752.71 49.42 96.13 0.65- 0.62 181 182124.73 30.81 91.16 0.62- 0.58 183 174697.96 29.85 97.81 ------------------------------------------------------------------------------------ 4.82- 0.58 1812 396635.75 55.30 96.36 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:31:18 2018 Sorting 1812 observations 84 unique observations with > 7.00 F2/sig(F2) 1812 observations in 3 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 Total number of frames 314 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 4 frame = 1 scale 1812 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 26 80 Total number of frames 80 1463 observations > 7.00 F2/sig(F2) 1463 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 26 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 15.9 (Out of 1463 removed 3 = 1460, unique = 92) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1460 observations in 3 runs Run # start # end # total # 1 0 27 28 2 0 24 53 3 0 26 80 Total number of frames 80 92 unique data precomputed (should be 92) 92 unique data with 1460 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 15.9 (Out of 1460 removed 0 = 1460, unique = 92) 92 unique data precomputed (should be 92) 92 unique data with 1460 observations RMS deviation of equivalent data = 0.14176 Rint = 0.11581 1 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11564, wR= 0.14399 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07524, wR= 0.09582, Acormin=0.793, Acormax=1.285, Acor_av=1.009 F test: Probability=1.000, F= 2.354 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07286, wR= 0.08903, Acormin=0.736, Acormax=1.326, Acor_av=0.972 F test: Probability=0.874, F= 1.064 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06142, wR= 0.07895, Acormin=0.708, Acormax=1.323, Acor_av=0.959 F test: Probability=1.000, F= 1.491 Trying model 4 (ne=4, no=1)... Results: Rint= 0.05914, wR= 0.07549, Acormin=0.709, Acormax=1.322, Acor_av=0.907 F test: Probability=0.911, F= 1.076 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04690, wR= 0.06365, Acormin=0.659, Acormax=1.313, Acor_av=0.882 F test: Probability=1.000, F= 1.702 Trying model 6 (ne=6, no=0)... Results: Rint= 0.05801, wR= 0.07561, Acormin=0.719, Acormax=1.319, Acor_av=0.958 F test: Probability=0.000, F= 0.652 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05657, wR= 0.07229, Acormin=0.698, Acormax=1.321, Acor_av=0.900 F test: Probability=0.000, F= 0.684 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04588, wR= 0.06152, Acormin=0.652, Acormax=1.331, Acor_av=0.891 F test: Probability=0.734, F= 1.035 Trying model 9 (ne=6, no=5)... Results: Rint= 0.03743, wR= 0.05212, Acormin=0.492, Acormax=1.194, Acor_av=0.789 F test: Probability=1.000, F= 1.542 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05539, wR= 0.07305, Acormin=0.686, Acormax=1.317, Acor_av=0.931 F test: Probability=0.000, F= 0.458 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05197, wR= 0.06839, Acormin=0.655, Acormax=1.280, Acor_av=0.870 F test: Probability=0.000, F= 0.519 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04336, wR= 0.05793, Acormin=0.499, Acormax=1.058, Acor_av=0.714 F test: Probability=0.000, F= 0.742 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03321, wR= 0.04797, Acormin=0.477, Acormax=1.170, Acor_av=0.771 F test: Probability=1.000, F= 1.255 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03031, wR= 0.04329, Acormin=0.505, Acormax=1.245, Acor_av=0.800 F test: Probability=0.999, F= 1.186 Final absorption model (ne=8, no=7): Rint= 0.03031, Acormin=0.505, Acormax=1.245, Acor_av=0.800 Combined refinement in use Rint: 0.11594 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14176 Using Levenberg-Marquardt: 0.00010 New wR= 0.03693 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11581 with corrections 0.02649 Rint for all data: 0.11594 with corrections 0.02671 3 observations identified as outliers and rejected Cycle 2 wR= 0.03338 Using Levenberg-Marquardt: 0.00001 New wR= 0.03165 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11551 with corrections 0.02316 Rint for all data: 0.11594 with corrections 0.02637 0 observations identified as outliers and rejected Cycle 3 wR= 0.03165 Using Levenberg-Marquardt: 0.00000 New wR= 0.03136 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11551 with corrections 0.02292 Rint for all data: 0.11594 with corrections 0.02602 0 observations identified as outliers and rejected Cycle 4 wR= 0.03136 Using Levenberg-Marquardt: 0.00000 New wR= 0.03120 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11551 with corrections 0.02276 Rint for all data: 0.11594 with corrections 0.02580 0 observations identified as outliers and rejected Cycle 5 wR= 0.03120 Using Levenberg-Marquardt: 0.00000 New wR= 0.03109 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11551 with corrections 0.02266 Rint for all data: 0.11594 with corrections 0.02565 0 observations identified as outliers and rejected Final wR= 0.03109 Final frame scales: Min= 0.8108 Max= 1.1207 Final absorption correction factors: Amin= 0.6381 Amax= 1.3150 PROFFIT INFO: Inet (after scale3 abspack): min=825.8931 max=5874394.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=132.3238 max=48102.5234 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/3 frame:1/109 1812 reflections read from tmp file 142 reflections are rejected (139 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 1 5 6 3 2 4 79 Initial Chi^2= 0.30307 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.64710 Current error model SIG(F2)^2 = 127.48*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 337.46*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 337.46*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5874394- 1215447 181 1973967.93 82.86 100.00 1202247- 694562 181 910630.86 38.43 100.00 689053- 297548 181 462228.05 37.27 100.00 297492- 175373 181 214508.75 26.86 100.00 175294- 142194 181 158436.11 18.79 100.00 142158- 98697 181 112580.29 13.41 100.00 98647- 77918 181 88901.41 11.20 100.00 77904- 5671 181 45332.57 7.95 88.95 5667- 3166 181 4145.57 2.83 16.57 3151- 826 183 2462.82 2.38 12.02 ------------------------------------------------------------------------------------ 5874394- 826 1812 396883.61 24.17 81.68 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 181 767867.92 54.73 96.69 1.39- 1.09 181 824757.58 43.74 89.50 1.09- 0.96 181 378383.55 25.38 82.32 0.96- 0.85 181 414215.77 23.66 83.98 0.85- 0.81 181 472344.94 25.30 90.06 0.81- 0.73 181 255745.55 15.44 69.61 0.73- 0.70 181 200754.54 13.30 73.48 0.70- 0.65 181 321478.70 17.86 88.95 0.65- 0.62 181 171659.65 11.41 72.93 0.62- 0.58 183 164199.01 11.07 69.40 ------------------------------------------------------------------------------------ 4.82- 0.58 1812 396883.61 24.17 81.68 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 181 767867.92 54.73 96.69 4.82- 1.09 362 796312.75 49.23 93.09 4.82- 0.96 543 657003.01 41.28 89.50 4.82- 0.85 724 596306.20 36.88 88.12 4.82- 0.81 905 571513.95 34.56 88.51 4.82- 0.73 1086 518885.88 31.37 85.36 4.82- 0.70 1267 473438.55 28.79 83.66 4.82- 0.65 1448 454443.57 27.43 84.32 4.82- 0.62 1629 423023.13 25.65 83.06 4.82- 0.58 1812 396883.61 24.17 81.68 ------------------------------------------------------------------------------------ 4.82- 0.58 1812 396883.61 24.17 81.68 Scale applied to data: s=0.170230 (maximum obs:5874394.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.026; Rsigma 0.026: data 1812 -> merged 110 With outlier rejection... Rint 0.022; Rsigma 0.027: data 1804 -> merged 110 Rejected total: 8, method kkm 7, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585863, 4.831154 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 9.60 100.00 96 1.61 - 1.21 10 10 16.30 100.00 163 1.17 - 1.01 10 10 21.30 100.00 213 0.99 - 0.89 10 10 20.80 100.00 208 0.88 - 0.81 10 10 20.60 100.00 206 0.81 - 0.74 10 10 17.30 100.00 173 0.73 - 0.71 10 10 19.70 100.00 197 0.70 - 0.66 10 10 16.30 100.00 163 0.66 - 0.64 10 10 14.80 100.00 148 0.63 - 0.60 10 10 14.60 100.00 146 --------------------------------------------------------------- 5.92 - 0.60 100 100 17.13 100.00 1713 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:31:17 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914808 5.917426 5.916140 60.0430 90.0569 60.0158 1666 Reflections read from file xs1714a.hkl; mean (I/sigma) = 24.47 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 819 887 826 840 1266 1120 1127 1666 N (int>3sigma) = 0 668 887 675 679 1115 937 932 1380 Mean intensity = 0.0 53.1 27.3 52.9 60.9 44.0 63.8 62.3 61.8 Mean int/sigma = 0.0 22.6 20.7 22.6 23.9 22.0 25.3 25.0 24.5 Lattice type: P chosen Volume: 146.48 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Unitcell: 5.915 5.915 5.916 119.98 90.06 119.94 Niggli form: a.a = 34.985 b.b = 34.986 c.c = 35.001 b.c = -17.485 a.c = -0.035 a.b = -17.458 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.083 CUBIC F-lattice R(int) = 0.194 [ 1512] Vol = 585.9 Cell: 8.362 8.372 8.370 89.97 89.99 90.02 Volume: 585.90 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 1244] Vol = 439.4 Cell: 5.915 5.915 14.494 89.98 90.04 119.94 Volume: 439.43 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 373] Vol = 439.4 Trigonal Cell: 5.915 5.915 14.494 89.98 90.04 119.94 Volume: 439.43 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.052 TETRAGONAL I-lattice R(int) = 0.152 [ 1275] Vol = 293.0 Cell: 5.921 5.918 8.362 89.97 90.01 90.01 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.039 TETRAGONAL I-lattice R(int) = 0.152 [ 1275] Vol = 293.0 Cell: 5.921 5.918 8.362 89.97 90.01 90.01 Volume: 292.95 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.154 [ 1228] Vol = 293.0 Cell: 5.921 8.362 5.918 89.97 89.99 89.99 Volume: 292.95 Matrix: 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.007 MONOCLINIC I-lattice R(int) = 0.126 [ 1013] Vol = 293.0 Cell: 8.362 5.921 5.918 90.01 90.03 89.99 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC C-lattice R(int) = 0.139 [ 1024] Vol = 293.0 Cell: 8.362 8.372 5.915 89.96 134.97 90.02 Volume: 292.95 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.104 [ 621] Vol = 146.5 Cell: 5.915 5.915 5.916 119.98 90.06 119.94 Volume: 146.48 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 887 0 1120 1127 1666 N (int>3sigma) = 0 0 0 0 887 0 937 934 1380 Mean intensity = 0.0 0.0 0.0 0.0 27.3 0.0 63.8 61.5 61.8 Mean int/sigma = 0.0 0.0 0.0 0.0 20.7 0.0 25.3 24.3 24.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.109 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 23 23 129 375 N I>3s 20 20 55 375 0.9 0.9 0.7 31.4 5.7 5.7 3.5 25.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.194 1403 Fd-3m 1 1 227 C N N N N 37 2284 0.197 1441 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361589 8.371788 8.369897 89.9700 89.9871 90.0248 ZERR 1.00 0.000354 0.004494 0.002020 0.0027 0.0020 0.0148 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4784962- 588287 407 402 27 14.9 1334099.77 56.62 0.019 0.022 574861- 135002 527 526 27 19.5 238969.20 26.25 0.027 0.031 119654- 40616 455 455 27 16.9 88467.74 11.21 0.040 0.052 11498- 1992 423 421 29 14.5 3948.15 2.86 0.147 0.188 ------------------------------------------------------------------------------------------- 4784962- 1992 1812 1804 110 16.4 390200.06 23.77 0.022 0.025 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 441 434 27 16.1 687084.53 43.77 0.020 0.022 0.015 1.01-0.78 556 555 28 19.8 375926.13 21.61 0.017 0.021 0.027 0.76-0.65 489 489 28 17.5 278378.25 16.11 0.025 0.030 0.039 0.65-0.59 326 326 27 12.1 186994.64 12.27 0.041 0.043 0.055 ------------------------------------------------------------------------------------------------------ inf-0.59 1812 1804 110 16.4 390200.06 23.77 0.022 0.025 0.027 inf-0.60 1719 1711 99 17.3 404430.90 24.51 0.022 0.024 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 434 27 27 100.0 16.1 687084.53 185.19 0.020 0.004 1.01-0.78 555 28 28 100.0 19.8 375926.13 100.59 0.017 0.006 0.76-0.65 489 28 28 100.0 17.5 278378.25 71.27 0.025 0.011 0.65-0.59 326 27 27 100.0 12.1 186994.64 49.81 0.041 0.018 -------------------------------------------------------------------------------------------- inf-0.59 1804 110 110 100.0 16.4 390200.06 103.82 0.022 0.007 inf-0.60 1711 99 99 100.0 17.3 404430.90 107.47 0.022 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:38:12 2018) ID: 2932; threads 39; handles 878; mem 518240.00 (1237700.00)kB; time: 1w 4d 23h 43m 43s MEMORY INFO: Memory PF:0.0, Ph:229.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.1,peak PF: 697.1, WS: 297.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:229.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.9,peak PF: 697.1, WS: 299.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:38:12 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000016 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000012 0.000011 ) 5.91502 ( 0.00095 ) 5.91640 ( 0.00095 ) 5.92265 ( 0.00074 ) 60.05206 ( 0.01483 ) 89.98756 ( 0.01145 ) 60.01743 ( 0.01674 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:38:12 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000017 0.000014 0.000014 ) -0.068858 -0.065594 -0.010716 ( 0.000019 0.000016 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000014 0.000012 0.000011 ) M - matrix: 0.021573 -0.014370 0.007199 ( 0.000005 0.000003 0.000003 ) -0.014370 0.028713 -0.014355 ( 0.000003 0.000004 0.000003 ) 0.007199 -0.014355 0.021551 ( 0.000003 0.000003 0.000004 ) unit cell: 5.9150(9) 5.9164(9) 5.9227(7) 60.052(15) 89.988(11) 60.017(17) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb PROFFITPEAK info: 316 peaks in the peak location table UB fit with 142 obs out of 155 (total:155,skipped:0) (91.61%) UB - matrix: -0.069721 0.031343 0.089421 ( 0.000090 0.000284 0.000172 ) -0.068809 -0.065744 -0.010227 ( 0.000113 0.000356 0.000216 ) 0.109025 -0.153049 0.116670 ( 0.000104 0.000326 0.000198 ) M - matrix: 0.021482 -0.014348 0.007189 ( 0.000030 0.000051 0.000032 ) -0.014348 0.028729 -0.014381 ( 0.000051 0.000112 0.000057 ) 0.007189 -0.014381 0.021713 ( 0.000032 0.000057 0.000056 ) unit cell: 5.928(14) 5.912(15) 5.888(10) 60.1(2) 90.03(16) 60.0(3) V = 146.1(5) UB fit with 142 obs out of 155 (total:155,skipped:0) (91.61%) UB - matrix: -0.069721 0.031343 0.089421 ( 0.000090 0.000284 0.000172 ) -0.068809 -0.065744 -0.010227 ( 0.000113 0.000356 0.000216 ) 0.109025 -0.153049 0.116670 ( 0.000104 0.000326 0.000198 ) M - matrix: 0.021482 -0.014348 0.007189 ( 0.000030 0.000051 0.000032 ) -0.014348 0.028729 -0.014381 ( 0.000051 0.000112 0.000057 ) 0.007189 -0.014381 0.021713 ( 0.000032 0.000057 0.000056 ) unit cell: 5.928(14) 5.912(15) 5.888(10) 60.1(2) 90.03(16) 60.0(3) V = 146.1(5) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.070012 0.031452 0.089277 ( 0.000088 0.000277 0.000167 ) -0.068945 -0.065834 -0.010423 ( 0.000108 0.000338 0.000203 ) 0.108771 -0.153518 0.116721 ( 0.000134 0.000421 0.000253 ) M - matrix: 0.021486 -0.014361 0.007164 ( 0.000035 0.000059 0.000037 ) -0.014361 0.028891 -0.014425 ( 0.000059 0.000138 0.000069 ) 0.007164 -0.014425 0.021703 ( 0.000037 0.000069 0.000066 ) UB fit with 140 obs out of 155 (total:155,skipped:0) (90.32%) unit cell: 5.922(14) 5.894(15) 5.890(10) 60.1(2) 89.97(16) 60.0(2) V = 145.6(5) UB fit with 140 obs out of 155 (total:155,skipped:0) (90.32%) UB - matrix: -0.070013 0.031447 0.089278 ( 0.000088 0.000276 0.000166 ) -0.068945 -0.065833 -0.010423 ( 0.000108 0.000338 0.000203 ) 0.108769 -0.153524 0.116722 ( 0.000134 0.000421 0.000254 ) M - matrix: 0.021486 -0.014362 0.007164 ( 0.000035 0.000059 0.000037 ) -0.014362 0.028893 -0.014426 ( 0.000059 0.000138 0.000069 ) 0.007164 -0.014426 0.021703 ( 0.000037 0.000069 0.000066 ) unit cell: 5.922(14) 5.894(15) 5.890(10) 60.0(2) 89.97(16) 60.0(2) V = 145.6(5) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.069883 0.031321 0.089392 ( 0.000084 0.000268 0.000158 ) -0.068875 -0.065602 -0.010338 ( 0.000107 0.000340 0.000201 ) 0.108513 -0.153560 0.116581 ( 0.000126 0.000402 0.000237 ) M - matrix: 0.021403 -0.014334 0.007116 ( 0.000033 0.000057 0.000035 ) -0.014334 0.028865 -0.014424 ( 0.000057 0.000132 0.000066 ) 0.007116 -0.014424 0.021689 ( 0.000035 0.000066 0.000062 ) UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) unit cell: 5.935(14) 5.903(14) 5.894(10) 60.0(2) 89.81(16) 59.9(2) V = 146.0(5) 155 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Run 4 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 269 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069883 0.031320 0.089393 ( 0.000084 0.000268 0.000158 ) -0.068875 -0.065601 -0.010338 ( 0.000107 0.000340 0.000201 ) 0.108513 -0.153560 0.116581 ( 0.000126 0.000402 0.000237 ) M - matrix: 0.021403 -0.014334 0.007116 ( 0.000033 0.000057 0.000035 ) -0.014334 0.028865 -0.014424 ( 0.000057 0.000132 0.000066 ) 0.007116 -0.014424 0.021689 ( 0.000035 0.000066 0.000062 ) UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) unit cell: 5.935(14) 5.903(14) 5.894(10) 60.0(2) 89.81(16) 59.9(2) V = 146.0(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb 1 of 99 peaks identified as outliers and rejected 98 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 98 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 98 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 1.41 | 10 | 1.053 ( 0.073) | 1.224 ( 0.556) | 1.234 ( 0.534) | 1.32- 1.12 | 10 | 1.036 ( 0.092) | 1.115 ( 0.203) | 1.110 ( 0.496) | 1.12- 0.96 | 10 | 1.034 ( 0.072) | 1.055 ( 0.074) | 0.995 ( 0.419) | 0.94- 0.84 | 10 | 1.052 ( 0.089) | 1.077 ( 0.095) | 1.081 ( 0.481) | 0.84- 0.78 | 10 | 1.022 ( 0.074) | 0.992 ( 0.095) | 1.222 ( 0.602) | 0.78- 0.73 | 10 | 1.008 ( 0.059) | 0.955 ( 0.077) | 1.049 ( 0.350) | 0.73- 0.69 | 10 | 1.010 ( 0.041) | 0.921 ( 0.103) | 1.273 ( 0.473) | 0.69- 0.67 | 10 | 0.991 ( 0.043) | 0.875 ( 0.046) | 1.111 ( 0.316) | 0.67- 0.62 | 10 | 0.944 ( 0.031) | 0.843 ( 0.051) | 1.123 ( 0.456) | 0.62- 0.59 | 8 | 0.922 ( 0.031) | 0.792 ( 0.035) | 1.385 ( 0.484) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 0.59 | 98 | 1.009 ( 0.076) | 0.989 ( 0.237) | 1.154 ( 0.480) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) UB - matrix: -0.070263 0.031187 0.088543 ( 0.000031 0.000112 0.000075 ) -0.068889 -0.065660 -0.010419 ( 0.000038 0.000135 0.000091 ) 0.108702 -0.152921 0.116066 ( 0.000018 0.000063 0.000042 ) M - matrix: 0.021499 -0.014291 0.007113 ( 0.000008 0.000014 0.000010 ) -0.014291 0.028669 -0.014303 ( 0.000014 0.000027 0.000015 ) 0.007113 -0.014303 0.021420 ( 0.000010 0.000015 0.000017 ) unit cell: 5.916(5) 5.919(5) 5.935(4) 59.94(8) 89.93(6) 60.08(10) V = 147.08(19) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.070242 0.031176 0.088560 ( 0.000031 0.000112 0.000075 ) -0.068883 -0.065637 -0.010400 ( 0.000038 0.000134 0.000090 ) 0.108667 -0.152929 0.116038 ( 0.000018 0.000065 0.000044 ) M - matrix: 0.021487 -0.014287 0.007105 ( 0.000008 0.000015 0.000010 ) -0.014287 0.028667 -0.014302 ( 0.000015 0.000027 0.000016 ) 0.007105 -0.014302 0.021416 ( 0.000010 0.000016 0.000017 ) UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) unit cell: 5.918(5) 5.920(5) 5.935(4) 59.93(8) 89.91(6) 60.07(9) V = 147.14(18) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 268 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 98 obs out of 98 (total:98,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb 2 of 98 peaks identified as outliers and rejected 96 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 96 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 96 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.41 | 10 | 1.042 ( 0.085) | 1.213 ( 0.544) | 1.143 ( 0.523) | 1.41- 1.12 | 10 | 1.028 ( 0.089) | 1.050 ( 0.097) | 1.202 ( 0.540) | 1.12- 0.96 | 10 | 1.033 ( 0.071) | 1.055 ( 0.075) | 0.951 ( 0.347) | 0.92- 0.84 | 10 | 1.037 ( 0.103) | 1.060 ( 0.116) | 0.967 ( 0.416) | 0.84- 0.78 | 10 | 1.038 ( 0.063) | 1.003 ( 0.096) | 1.261 ( 0.595) | 0.78- 0.73 | 10 | 1.007 ( 0.058) | 0.955 ( 0.077) | 1.111 ( 0.363) | 0.72- 0.69 | 10 | 0.997 ( 0.048) | 0.896 ( 0.108) | 1.194 ( 0.501) | 0.69- 0.66 | 10 | 0.987 ( 0.043) | 0.881 ( 0.048) | 1.162 ( 0.402) | 0.65- 0.61 | 10 | 0.944 ( 0.037) | 0.827 ( 0.045) | 1.115 ( 0.417) | 0.60- 0.59 | 6 | 0.908 ( 0.036) | 0.795 ( 0.037) | 1.167 ( 0.327) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.59 | 96 | 1.006 ( 0.079) | 0.981 ( 0.226) | 1.126 ( 0.466) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.4 | 142 | 1.116 ( 0.114) | 1.247 ( 0.459) | 1.132 ( 0.529) | 13.5-19.2 | 142 | 1.080 ( 0.055) | 1.123 ( 0.238) | 1.213 ( 0.525) | 19.2-23.2 | 142 | 1.073 ( 0.077) | 1.151 ( 0.394) | 1.189 ( 0.509) | 23.3-27.2 | 142 | 1.033 ( 0.083) | 1.084 ( 0.313) | 1.210 ( 0.588) | 27.2-30.9 | 142 | 1.015 ( 0.079) | 1.001 ( 0.180) | 1.228 ( 0.511) | 30.9-33.8 | 142 | 0.983 ( 0.088) | 0.927 ( 0.103) | 1.178 ( 0.509) | 33.8-36.9 | 142 | 0.967 ( 0.080) | 0.901 ( 0.099) | 1.182 ( 0.500) | 36.9-39.7 | 142 | 0.950 ( 0.096) | 0.883 ( 0.154) | 1.177 ( 0.550) | 39.7-42.8 | 142 | 0.924 ( 0.087) | 0.836 ( 0.085) | 1.174 ( 0.506) | 42.8-49.9 | 145 | 0.937 ( 0.084) | 0.820 ( 0.069) | 1.160 ( 0.449) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1423 | 1.008 ( 0.106) | 0.997 ( 0.283) | 1.184 ( 0.519) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0097 b=1.26 e3 dimension: a=0.0021 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 9708196 lp-corr: 2806008 PROFFITPEAK - Finished at Tue Mar 27 14:38:26 2018 PROFFITMAIN - Started at Tue Mar 27 14:38:26 2018 OTKP changes: 1423 2 3 4 OTKP changes: 1423 2 3 4 UB - matrix: -0.070215 0.031085 0.088914 ( 0.000014 0.000013 0.000013 ) -0.068764 -0.065854 -0.010511 ( 0.000015 0.000013 0.000013 ) 0.109182 -0.153053 0.116329 ( 0.000012 0.000011 0.000011 ) M - matrix: 0.021579 -0.014365 0.007181 ( 0.000004 0.000003 0.000003 ) -0.014365 0.028728 -0.014348 ( 0.000003 0.000004 0.000003 ) 0.007181 -0.014348 0.021549 ( 0.000003 0.000003 0.000003 ) UB fit with 1423 obs out of 1423 (total:1423,skipped:0) (100.00%) unit cell: 5.9116(8) 5.9135(8) 5.9145(7) 60.044(13) 90.024(10) 60.023(14) V = 146.32(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070052 0.030666 0.088960 ( 0.000028 0.000028 0.000016 ) -0.068242 -0.066139 -0.010508 ( 0.000025 0.000025 0.000014 ) 0.109072 -0.153058 0.115976 ( 0.000025 0.000024 0.000014 ) M - matrix: 0.021461 -0.014329 0.007135 ( 0.000008 0.000006 0.000004 ) -0.014329 0.028741 -0.014328 ( 0.000006 0.000008 0.000004 ) 0.007135 -0.014328 0.021475 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9279(14) 5.9138(14) 5.9248(11) 60.02(2) 89.967(18) 60.00(2) V = 146.94(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070327 0.030938 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068414 -0.066125 -0.010692 ( 0.000024 0.000023 0.000013 ) 0.109330 -0.153285 0.116370 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014411 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014411 0.028826 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014384 0.021542 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9074(13) 5.9181(10) 60.05(2) 90.074(16) 60.00(2) V = 146.27(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.793) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070327 0.030938 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068414 -0.066125 -0.010692 ( 0.000024 0.000023 0.000013 ) 0.109330 -0.153285 0.116370 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014411 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014411 0.028826 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014384 0.021542 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9074(13) 5.9181(10) 60.05(2) 90.074(16) 60.00(2) V = 146.27(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070327 0.030938 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068414 -0.066125 -0.010692 ( 0.000024 0.000023 0.000013 ) 0.109330 -0.153285 0.116370 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014411 0.007209 ( 0.000007 0.000005 0.000004 ) -0.014411 0.028826 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007209 -0.014384 0.021542 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9074(13) 5.9181(10) 60.05(2) 90.074(16) 60.00(2) V = 146.27(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031348 0.088634 ( 0.000026 0.000022 0.000027 ) -0.068579 -0.065999 -0.010237 ( 0.000031 0.000027 0.000033 ) 0.108991 -0.152649 0.116248 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021540 -0.014318 0.007131 ( 0.000007 0.000005 0.000005 ) -0.014318 0.028640 -0.014291 ( 0.000005 0.000007 0.000005 ) 0.007131 -0.014291 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(16) 5.9211(16) 5.9225(13) 60.03(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070356 0.031198 0.088847 ( 0.000023 0.000020 0.000025 ) -0.068785 -0.065859 -0.010345 ( 0.000030 0.000026 0.000032 ) 0.109166 -0.153155 0.116577 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014384 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028767 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014401 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9096(16) 5.9164(16) 5.9146(12) 59.94(2) 89.944(19) 60.01(3) V = 146.17(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.793) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070356 0.031198 0.088847 ( 0.000023 0.000020 0.000025 ) -0.068785 -0.065859 -0.010345 ( 0.000030 0.000026 0.000032 ) 0.109166 -0.153155 0.116577 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014384 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028767 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014401 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9096(16) 5.9164(16) 5.9146(12) 59.94(2) 89.944(19) 60.01(3) V = 146.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070356 0.031198 0.088847 ( 0.000023 0.000020 0.000025 ) -0.068785 -0.065859 -0.010345 ( 0.000030 0.000026 0.000032 ) 0.109166 -0.153155 0.116577 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014384 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028767 -0.014401 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014401 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9096(16) 5.9164(16) 5.9146(12) 59.94(2) 89.944(19) 60.01(3) V = 146.17(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 96 obs out of 96 (total:96,skipped:0) (100.00%) UB - matrix: -0.070201 0.031251 0.088545 ( 0.000030 0.000108 0.000072 ) -0.068860 -0.065779 -0.010344 ( 0.000038 0.000135 0.000090 ) 0.108873 -0.152851 0.116177 ( 0.000012 0.000045 0.000030 ) M - matrix: 0.021523 -0.014306 0.007145 ( 0.000007 0.000013 0.000009 ) -0.014306 0.028667 -0.014310 ( 0.000013 0.000023 0.000013 ) 0.007145 -0.014310 0.021444 ( 0.000009 0.000013 0.000015 ) unit cell: 5.914(5) 5.918(5) 5.931(4) 59.99(8) 90.01(6) 60.09(9) V = 146.95(18) OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 OTKP changes: 96 1 1 1 UB - matrix: -0.070264 0.031280 0.088841 ( 0.000029 0.000102 0.000069 ) -0.068771 -0.066097 -0.010219 ( 0.000036 0.000130 0.000087 ) 0.109098 -0.153126 0.116473 ( 0.000012 0.000042 0.000028 ) M - matrix: 0.021569 -0.014358 0.007167 ( 0.000007 0.000013 0.000009 ) -0.014358 0.028795 -0.014381 ( 0.000013 0.000022 0.000013 ) 0.007167 -0.014381 0.021563 ( 0.000009 0.000013 0.000014 ) UB fit with 96 obs out of 96 (total:96,skipped:0) (100.00%) unit cell: 5.909(5) 5.906(5) 5.915(3) 59.98(8) 89.99(6) 60.07(9) V = 146.09(17) Run 4 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.793) HKL list info: 263 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070264 0.031280 0.088841 ( 0.000029 0.000102 0.000069 ) -0.068771 -0.066097 -0.010219 ( 0.000036 0.000130 0.000087 ) 0.109098 -0.153126 0.116473 ( 0.000012 0.000042 0.000028 ) M - matrix: 0.021569 -0.014358 0.007167 ( 0.000007 0.000013 0.000009 ) -0.014358 0.028795 -0.014381 ( 0.000013 0.000022 0.000013 ) 0.007167 -0.014381 0.021563 ( 0.000009 0.000013 0.000014 ) UB fit with 96 obs out of 96 (total:96,skipped:0) (100.00%) unit cell: 5.909(5) 5.906(5) 5.915(3) 59.98(8) 89.99(6) 60.07(9) V = 146.09(17) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070192 0.031085 0.088838 ( 0.000015 0.000013 0.000013 ) -0.068756 -0.065745 -0.010574 ( 0.000017 0.000015 0.000015 ) 0.109158 -0.153045 0.116369 ( 0.000012 0.000011 0.000011 ) M - matrix: 0.021570 -0.014368 0.007194 ( 0.000004 0.000003 0.000003 ) -0.014368 0.028712 -0.014353 ( 0.000003 0.000004 0.000003 ) 0.007194 -0.014353 0.021546 ( 0.000003 0.000003 0.000003 ) UB fit with 1423 obs out of 1423 (total:1423,skipped:0) (100.00%) unit cell: 5.9149(9) 5.9177(9) 5.9169(7) 60.037(14) 90.046(11) 60.015(16) V = 146.50(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 55 reflections under beam stop or inside a detector rejection region 12 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof 1953 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:38:30 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.793) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.793) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.793) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2940429.5635 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4704687.5000 PROFFIT INFO: sig(Inet): min=96.3819 max=47450.0938 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.48 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 12 71 180 400 442 762 1279 1777 1953 Percent 0.0 0.0 0.6 3.6 9.2 20.5 22.6 39.0 65.5 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1953 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1953 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4704688- 1228602 195 1944095.95 124.00 100.00 1226490- 719356 195 931161.66 107.05 100.00 716966- 277940 195 466002.33 96.11 100.00 276448- 177965 195 214922.66 73.97 100.00 177372- 134098 195 156869.46 51.48 100.00 133259- 102069 195 116619.27 37.51 100.00 101974- 77925 195 89846.93 30.38 100.00 77845- 5854 195 44320.73 20.15 100.00 5827- 3216 195 4275.72 5.57 97.95 3205- 924 198 2388.94 4.15 66.16 ------------------------------------------------------------------------------------ 4704688- 924 1953 396444.13 54.96 96.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 195 681907.65 86.33 98.97 1.41- 1.07 195 609297.12 68.78 98.46 1.07- 0.96 195 449960.17 62.36 96.92 0.96- 0.83 195 447826.50 56.91 95.38 0.83- 0.75 195 392485.97 56.51 96.92 0.75- 0.69 195 310060.33 48.70 96.41 0.69- 0.63 195 333178.41 51.28 96.92 0.63- 0.58 195 307184.15 47.14 95.38 0.58- 0.52 195 237798.68 38.59 93.33 0.52- 0.40 198 197798.37 33.34 94.95 ------------------------------------------------------------------------------------ 5.26- 0.40 1953 396444.13 54.96 96.36 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:38:30 2018 Sorting 1953 observations 238 unique observations with > 7.00 F2/sig(F2) 1953 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 23 337 Total number of frames 337 Maximum number of 238 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 1953 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 11 171 Total number of frames 171 1572 observations > 7.00 F2/sig(F2) 1572 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 11 171 Total number of frames 171 Removing 'redundancy=1' reflections Average redundancy: 6.6 (Out of 1572 removed 48 = 1524, unique = 232) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1524 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 11 171 Total number of frames 171 232 unique data precomputed (should be 232) 232 unique data with 1524 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 6.6 (Out of 1524 removed 0 = 1524, unique = 232) 232 unique data precomputed (should be 232) 232 unique data with 1524 observations RMS deviation of equivalent data = 0.71026 Rint = 0.67310 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.65467, wR= 4.06549 Trying model 1 (ne=2, no=0)... Results: Rint= 0.73248, wR= 3.03949, Acormin=-0.016, Acormax=2.042, Acor_av=0.631 F test: Probability=0.000, F= 0.796 Trying model 2 (ne=2, no=1)... Results: Rint= 0.91198, wR= 2.86013, Acormin=-0.428, Acormax=1.917, Acor_av=0.346 F test: Probability=0.000, F= 0.512 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75485, wR= 2.36122, Acormin=-0.158, Acormax=2.209, Acor_av=0.501 F test: Probability=0.000, F= 0.744 Trying model 4 (ne=4, no=1)... Results: Rint= 0.90809, wR= 2.42608, Acormin=-0.544, Acormax=2.022, Acor_av=0.268 F test: Probability=0.000, F= 0.513 Trying model 5 (ne=4, no=3)... Results: Rint= 0.97060, wR= 2.11098, Acormin=-1.180, Acormax=1.554, Acor_av=0.087 F test: Probability=0.000, F= 0.446 Trying model 6 (ne=6, no=0)... Results: Rint= 0.79577, wR= 2.41002, Acormin=-0.244, Acormax=2.823, Acor_av=0.432 F test: Probability=0.000, F= 0.663 Trying model 7 (ne=6, no=1)... Results: Rint= 0.94011, wR= 2.48762, Acormin=-0.625, Acormax=2.284, Acor_av=0.202 F test: Probability=0.000, F= 0.474 Trying model 8 (ne=6, no=3)... Results: Rint= 0.96555, wR= 2.44585, Acormin=-1.217, Acormax=1.604, Acor_av=0.066 F test: Probability=0.000, F= 0.446 Trying model 9 (ne=6, no=5)... Results: Rint= 1.03359, wR= 2.37419, Acormin=-0.669, Acormax=3.008, Acor_av=0.029 F test: Probability=0.000, F= 0.386 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86282, wR= 2.06610, Acormin=-0.638, Acormax=2.988, Acor_av=0.333 F test: Probability=0.000, F= 0.556 Trying model 11 (ne=8, no=1)... Results: Rint= 1.00243, wR= 2.00880, Acormin=-1.100, Acormax=1.295, Acor_av=0.031 F test: Probability=0.000, F= 0.411 Trying model 12 (ne=8, no=3)... Results: Rint= 0.97922, wR= 1.46043, Acormin=-0.039, Acormax=0.079, Acor_av=0.002 F test: Probability=0.000, F= 0.428 Trying model 13 (ne=8, no=5)... Results: Rint= 0.98270, wR= 1.46721, Acormin=-0.040, Acormax=0.087, Acor_av=0.002 F test: Probability=0.000, F= 0.421 Trying model 14 (ne=8, no=7)... Results: Rint= 0.99908, wR= 1.41296, Acormin=-0.041, Acormax=0.140, Acor_av=0.001 F test: Probability=0.000, F= 0.403 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.84096 There are 171 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 175 pars with 15400 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71026 Using Levenberg-Marquardt: 0.00010 New wR= 0.69032 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67310 with corrections 0.64143 Rint for all data: 0.84096 with corrections 0.81927 9 observations identified as outliers and rejected Cycle 2 wR= 0.66790 Using Levenberg-Marquardt: 0.00001 New wR= 0.84020 Using Levenberg-Marquardt: 0.00010 New wR= 0.81336 Using Levenberg-Marquardt: 0.00100 New wR= 0.68996 Using Levenberg-Marquardt: 0.01000 New wR= 0.66401 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65272 with corrections 0.63121 Rint for all data: 0.84096 with corrections 0.82601 10 observations identified as outliers and rejected Cycle 3 wR= 0.62469 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62324 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63976 with corrections 0.62022 Rint for all data: 0.84096 with corrections 0.82843 5 observations identified as outliers and rejected Cycle 4 wR= 0.61559 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61493 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63492 with corrections 0.61793 Rint for all data: 0.84096 with corrections 0.83008 8 observations identified as outliers and rejected Cycle 5 wR= 0.59783 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.59664 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.63183 with corrections 0.62236 Rint for all data: 0.84096 with corrections 0.83398 4 observations identified as outliers and rejected Final wR= 0.59664 Final frame scales: Min= 0.7687 Max= 3.2410 Final absorption correction factors: Amin= 0.4216 Amax= 1.4957 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=709.6323 max=5498554.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=112.9113 max=75774.2500 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/108 1952 reflections read from tmp file 1511 reflections are rejected (1424 as outliers, 87 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 89 36 14 8 6 2 0 1 Initial Chi^2= 0.76911 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.56101 Current error model SIG(F2)^2 = 465.57*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 261.19*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 261.19*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5498554- 1184918 195 1980370.99 91.32 100.00 1183117- 646651 195 889524.83 46.50 100.00 641976- 273166 195 435891.86 41.44 100.00 272981- 175279 195 216861.63 31.14 100.00 175182- 133167 195 151710.15 20.24 100.00 133061- 96984 195 116048.00 16.60 100.00 96919- 68856 195 82766.67 13.00 100.00 68755- 5878 195 38982.04 9.32 91.79 5811- 2985 195 4014.27 3.21 38.97 2969- 710 197 2229.58 2.71 25.89 ------------------------------------------------------------------------------------ 5498554- 710 1952 391440.81 27.52 85.60 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 195 782428.61 59.03 96.41 1.41- 1.07 195 612951.01 41.72 93.33 1.07- 0.96 195 490673.69 30.67 91.28 0.96- 0.83 195 447833.87 27.83 83.08 0.83- 0.75 195 365997.29 24.93 84.62 0.75- 0.69 195 298168.29 20.53 83.59 0.69- 0.63 195 296853.65 21.14 81.54 0.63- 0.58 195 285345.00 19.43 83.08 0.57- 0.52 195 191704.28 16.09 78.97 0.52- 0.40 197 144980.21 13.99 80.20 ------------------------------------------------------------------------------------ 5.26- 0.40 1952 391440.81 27.52 85.60 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 195 782428.61 59.03 96.41 5.26- 1.07 390 697689.81 50.37 94.87 5.26- 0.96 585 628684.44 43.81 93.68 5.26- 0.83 780 583471.80 39.81 91.03 5.26- 0.75 975 539976.90 36.84 89.74 5.26- 0.69 1170 499675.46 34.12 88.72 5.26- 0.63 1365 470700.92 32.27 87.69 5.26- 0.58 1560 447531.43 30.66 87.12 5.26- 0.52 1755 419106.19 29.04 86.21 5.26- 0.40 1952 391440.81 27.52 85.60 ------------------------------------------------------------------------------------ 5.26- 0.40 1952 391440.81 27.52 85.60 Scale applied to data: s=0.181866 (maximum obs:5498554.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.834; Rsigma 0.023: data 1952 -> merged 302 With outlier rejection... Rint 0.745; Rsigma 0.024: data 1805 -> merged 302 Rejected total: 147, method kkm 135, method Blessing 12 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404319, 5.271675 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.46 15 15 9.73 100.00 146 1.46 - 1.12 15 15 14.27 100.00 214 1.08 - 0.96 15 15 12.33 100.00 185 0.96 - 0.86 15 15 11.00 100.00 165 0.86 - 0.79 15 15 9.73 100.00 146 0.79 - 0.73 15 15 8.60 100.00 129 0.73 - 0.69 15 15 7.40 100.00 111 0.69 - 0.65 15 15 7.07 100.00 106 0.65 - 0.63 15 15 4.87 100.00 73 0.63 - 0.60 21 21 4.90 100.00 103 --------------------------------------------------------------- 5.91 - 0.60 156 156 8.83 100.00 1378 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:38:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914936 5.917667 5.916898 60.0372 90.0459 60.0146 1805 Reflections read from file xs1714a.hkl; mean (I/sigma) = 26.78 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 888 956 896 909 1370 1212 1220 1805 N (int>3sigma) = 0 756 956 764 764 1238 1046 1038 1539 Mean intensity = 0.0 58.4 28.8 57.9 65.4 47.9 69.4 65.7 66.3 Mean int/sigma = 0.0 25.4 22.6 25.0 26.3 24.3 27.9 27.0 26.8 Lattice type: P chosen Volume: 146.50 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Unitcell: 5.915 5.916 5.917 119.99 90.05 119.94 Niggli form: a.a = 34.986 b.b = 34.997 c.c = 35.010 b.c = -17.494 a.c = -0.028 a.b = -17.465 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.192 [ 1652] Vol = 586.0 Cell: 8.363 8.372 8.370 89.97 89.98 90.02 Volume: 586.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1385] Vol = 439.5 Cell: 5.916 5.915 14.495 89.98 90.03 119.94 Volume: 439.51 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 417] Vol = 439.5 Trigonal Cell: 5.916 5.915 14.495 89.98 90.03 119.94 Volume: 439.51 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.047 TETRAGONAL I-lattice R(int) = 0.164 [ 1413] Vol = 293.0 Cell: 5.921 5.918 8.363 89.97 90.00 90.02 Volume: 293.01 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.040 TETRAGONAL I-lattice R(int) = 0.164 [ 1413] Vol = 293.0 Cell: 5.921 5.918 8.363 89.97 90.00 90.02 Volume: 293.01 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.162 [ 1366] Vol = 293.0 Cell: 5.921 8.363 5.918 89.97 89.98 90.00 Volume: 293.01 Matrix: 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.127 [ 1114] Vol = 293.0 Cell: 8.363 5.921 5.918 90.02 90.03 90.00 Volume: 293.01 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC C-lattice R(int) = 0.143 [ 1146] Vol = 293.0 Cell: 8.363 8.372 5.915 89.97 134.97 90.02 Volume: 293.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.119 [ 698] Vol = 146.5 Cell: 5.915 5.916 5.917 119.99 90.05 119.94 Volume: 146.50 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 956 0 1212 1222 1805 N (int>3sigma) = 0 0 0 0 956 0 1046 1045 1539 Mean intensity = 0.0 0.0 0.0 0.0 28.8 0.0 69.4 64.8 66.3 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 27.9 26.5 26.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.145 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 131 412 N I>3s 17 17 72 412 0.8 0.8 0.7 33.8 5.6 5.6 3.7 27.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.191 1540 Fd-3m 1 1 227 C N N N N 37 2284 0.193 1578 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363018 8.372047 8.369721 89.9709 89.9810 90.0180 ZERR 1.00 0.000327 0.004162 0.001876 0.0025 0.0019 0.0137 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2960460- 679652 314 290 30 9.7 1010345.56 55.72 0.671 0.630 656537- 506694 208 199 30 6.6 543869.24 36.05 0.821 0.729 503247- 389737 264 249 30 8.3 408144.03 30.90 0.932 0.931 388277- 284403 223 200 30 6.7 296720.14 22.89 0.854 0.832 283515- 203884 209 176 30 5.9 167297.74 18.39 0.744 0.803 202649- 129973 256 236 30 7.9 146188.40 18.93 0.639 0.711 123846- 83628 188 178 30 5.9 101133.37 14.08 0.477 0.444 82156- 60741 120 112 30 3.7 73730.67 12.09 0.377 0.252 60205- 38483 91 87 30 2.9 52299.23 9.43 0.583 0.449 36529- 1386 79 78 32 2.4 15719.95 4.42 0.829 0.811 ------------------------------------------------------------------------------------------- 2960460- 1386 1952 1805 302 6.0 364644.16 26.78 0.745 0.712 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 388 360 30 12.0 653395.52 49.38 0.739 0.791 0.014 1.08-0.86 375 357 30 11.9 457069.80 28.87 0.876 0.992 0.022 0.86-0.73 296 273 31 8.8 331235.61 23.12 0.702 0.626 0.029 0.72-0.65 231 208 31 6.7 261216.87 20.08 0.688 0.674 0.032 0.65-0.60 181 162 30 5.4 216067.69 16.87 0.768 0.783 0.036 0.60-0.56 164 151 33 4.6 208458.58 17.23 0.530 0.482 0.038 0.56-0.52 127 114 31 3.7 205420.11 17.35 0.634 0.629 0.039 0.52-0.49 102 93 30 3.1 141619.18 13.38 0.542 0.384 0.045 0.49-0.45 57 56 30 1.9 147796.61 14.20 0.401 0.288 0.045 0.45-0.40 31 31 26 1.2 118731.41 13.31 0.386 0.386 0.048 ------------------------------------------------------------------------------------------------------ inf-0.40 1952 1805 302 6.0 364644.16 26.78 0.745 0.712 0.024 inf-0.60 1491 1378 156 8.8 424022.09 30.32 0.767 0.787 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 360 30 30 100.0 12.0 653395.52 193.76 0.739 0.005 1.08-0.86 357 30 30 100.0 11.9 457069.80 119.93 0.876 0.009 0.86-0.73 273 31 31 100.0 8.8 331235.61 82.96 0.702 0.013 0.72-0.65 208 31 31 100.0 6.7 261216.87 62.53 0.688 0.016 0.65-0.60 162 30 30 100.0 5.4 216067.69 51.52 0.768 0.021 0.60-0.56 151 38 33 86.8 4.6 208458.58 43.68 0.530 0.020 0.56-0.52 114 37 31 83.8 3.7 205420.11 42.62 0.634 0.024 0.52-0.49 93 48 30 62.5 3.1 141619.18 29.10 0.542 0.029 0.49-0.45 56 62 30 48.4 1.9 147796.61 22.30 0.401 0.037 0.45-0.40 31 119 26 21.8 1.2 118731.41 15.55 0.386 0.036 -------------------------------------------------------------------------------------------- inf-0.40 1805 457 302 66.1 6.0 364644.16 95.55 0.745 0.014 inf-0.60 1378 156 156 100.0 8.8 424022.09 114.44 0.767 0.011 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 -1.0 2.0 -1.0 1.0 0.0 -1.0 No constraint UB - matrix: -0.024864 0.015542 -0.079514 ( 0.000008 0.000006 0.000008 ) 0.072538 -0.032872 -0.029090 ( 0.000010 0.000008 0.000009 ) -0.036240 -0.076522 -0.003606 ( 0.000007 0.000005 0.000006 ) M - matrix: 0.007193 0.000002 -0.000002 ( 0.000002 0.000001 0.000001 ) 0.000002 0.007178 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000002 -0.000004 0.007182 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024864 0.015542 -0.079514 ( 0.000008 0.000006 0.000008 ) 0.072538 -0.032872 -0.029090 ( 0.000010 0.000008 0.000009 ) -0.036240 -0.076522 -0.003606 ( 0.000007 0.000005 0.000006 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3630(8) 8.3721(6) 8.3698(8) 89.971(7) 89.981(8) 90.018(7) V = 586.02(9) unit cell: 8.3683(2) 8.3683(2) 8.3683(2) 90.0 90.0 90.0 V = 586.02(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.793) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.793) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.793) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2940429.5635 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4704687.5000 PROFFIT INFO: sig(Inet): min=96.3819 max=47450.0938 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.48 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 24 142 360 800 884 1524 2558 3554 3906 Percent 0.0 0.0 0.6 3.6 9.2 20.5 22.6 39.0 65.5 91.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 1953 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 1953 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4704688- 1228602 195 1944095.95 124.00 100.00 1226490- 719356 195 931161.66 107.05 100.00 716966- 277940 195 466002.33 96.11 100.00 276448- 177965 195 214922.66 73.97 100.00 177372- 134098 195 156869.46 51.48 100.00 133259- 102069 195 116619.27 37.51 100.00 101974- 77925 195 89846.93 30.38 100.00 77845- 5854 195 44320.73 20.15 100.00 5827- 3216 195 4275.72 5.57 97.95 3205- 924 198 2388.94 4.15 66.16 ------------------------------------------------------------------------------------ 4704688- 924 1953 396444.13 54.96 96.36 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 195 725270.22 91.77 100.00 1.39- 1.09 195 822714.79 69.53 100.00 1.09- 0.96 195 384081.25 67.66 97.95 0.96- 0.85 195 415000.14 64.62 95.90 0.85- 0.80 195 460566.88 68.27 99.49 0.80- 0.73 195 261669.91 42.25 99.49 0.73- 0.70 195 210306.25 36.26 86.15 0.70- 0.65 195 339320.05 49.94 96.92 0.65- 0.62 195 174739.01 29.95 90.26 0.62- 0.58 198 174192.05 29.75 97.47 ------------------------------------------------------------------------------------ 4.82- 0.58 1953 396444.13 54.96 96.36 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:38:31 2018 Sorting 1953 observations 84 unique observations with > 7.00 F2/sig(F2) 1953 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 23 337 Total number of frames 337 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 1953 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 4 69 Total number of frames 69 1572 observations > 7.00 F2/sig(F2) 1572 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 4 69 Total number of frames 69 Removing 'redundancy=1' reflections Average redundancy: 17.1 (Out of 1572 removed 3 = 1569, unique = 92) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1569 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 4 69 Total number of frames 69 92 unique data precomputed (should be 92) 92 unique data with 1569 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 17.1 (Out of 1569 removed 0 = 1569, unique = 92) 92 unique data precomputed (should be 92) 92 unique data with 1569 observations RMS deviation of equivalent data = 0.14111 Rint = 0.11437 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11392, wR= 0.14071 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07837, wR= 0.09806, Acormin=0.786, Acormax=1.264, Acor_av=0.997 F test: Probability=1.000, F= 2.106 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07515, wR= 0.09156, Acormin=0.750, Acormax=1.304, Acor_av=0.966 F test: Probability=0.942, F= 1.085 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06393, wR= 0.08245, Acormin=0.718, Acormax=1.299, Acor_av=0.949 F test: Probability=1.000, F= 1.494 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06240, wR= 0.07891, Acormin=0.680, Acormax=1.282, Acor_av=0.897 F test: Probability=0.813, F= 1.048 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05106, wR= 0.06820, Acormin=0.646, Acormax=1.277, Acor_av=0.859 F test: Probability=1.000, F= 1.557 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06146, wR= 0.07957, Acormin=0.742, Acormax=1.305, Acor_av=0.949 F test: Probability=0.000, F= 0.689 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05974, wR= 0.07634, Acormin=0.676, Acormax=1.302, Acor_av=0.889 F test: Probability=0.000, F= 0.728 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04936, wR= 0.06543, Acormin=0.627, Acormax=1.297, Acor_av=0.870 F test: Probability=0.868, F= 1.061 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04196, wR= 0.05681, Acormin=0.515, Acormax=1.183, Acor_av=0.788 F test: Probability=1.000, F= 1.456 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05970, wR= 0.07751, Acormin=0.702, Acormax=1.293, Acor_av=0.922 F test: Probability=0.000, F= 0.495 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05485, wR= 0.07118, Acormin=0.643, Acormax=1.242, Acor_av=0.855 F test: Probability=0.000, F= 0.586 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04666, wR= 0.06119, Acormin=0.501, Acormax=1.035, Acor_av=0.704 F test: Probability=0.000, F= 0.805 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03696, wR= 0.05131, Acormin=0.477, Acormax=1.140, Acor_av=0.760 F test: Probability=1.000, F= 1.273 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03406, wR= 0.04732, Acormin=0.472, Acormax=1.207, Acor_av=0.783 F test: Probability=0.998, F= 1.165 Final absorption model (ne=8, no=7): Rint= 0.03406, Acormin=0.472, Acormax=1.207, Acor_av=0.783 Combined refinement in use Rint: 0.11450 There are 69 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 148 pars with 11026 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.14111 Using Levenberg-Marquardt: 0.00010 New wR= 0.03882 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11437 with corrections 0.02821 Rint for all data: 0.11450 with corrections 0.02843 3 observations identified as outliers and rejected Cycle 2 wR= 0.03544 Using Levenberg-Marquardt: 0.00001 New wR= 0.03384 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11409 with corrections 0.02513 Rint for all data: 0.11450 with corrections 0.02822 0 observations identified as outliers and rejected Cycle 3 wR= 0.03384 Using Levenberg-Marquardt: 0.00000 New wR= 0.03358 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11409 with corrections 0.02508 Rint for all data: 0.11450 with corrections 0.02810 0 observations identified as outliers and rejected Cycle 4 wR= 0.03358 Using Levenberg-Marquardt: 0.00000 New wR= 0.03346 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11409 with corrections 0.02506 Rint for all data: 0.11450 with corrections 0.02803 0 observations identified as outliers and rejected Cycle 5 wR= 0.03346 Using Levenberg-Marquardt: 0.00000 New wR= 0.03338 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11409 with corrections 0.02505 Rint for all data: 0.11450 with corrections 0.02798 0 observations identified as outliers and rejected Final wR= 0.03338 Final frame scales: Min= 0.8599 Max= 1.1547 Final absorption correction factors: Amin= 0.5984 Amax= 1.3027 PROFFIT INFO: Inet (after scale3 abspack): min=827.9717 max=5965739.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=114.0178 max=48049.6055 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 1953 reflections read from tmp file 179 reflections are rejected (176 as outliers, 3 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 3 4 6 2 3 0 83 Initial Chi^2= 0.30706 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.63317 Current error model SIG(F2)^2 = 131.08*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 345.14*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 345.14*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5965740- 1224353 195 1964105.45 81.79 100.00 1211391- 690766 195 905915.93 37.79 100.00 685722- 294400 195 464025.64 37.72 100.00 292895- 174666 195 215692.03 26.82 100.00 174510- 141026 195 157539.73 18.47 100.00 140609- 98475 195 112550.80 13.24 100.00 98309- 77664 195 88832.87 11.03 100.00 77372- 5565 195 44498.55 7.71 87.69 5524- 3135 195 4112.91 2.77 15.38 3133- 828 198 2420.66 2.35 11.11 ------------------------------------------------------------------------------------ 5965740- 828 1953 395364.93 23.94 81.31 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 195 759153.11 54.79 96.41 1.39- 1.09 195 828334.97 43.46 89.23 1.09- 0.96 195 384933.73 25.40 82.05 0.96- 0.85 195 416945.60 23.40 83.59 0.85- 0.80 195 449796.38 24.29 88.72 0.80- 0.73 195 256324.70 15.30 69.23 0.73- 0.70 195 204858.90 13.21 73.33 0.70- 0.65 195 325674.16 17.82 90.26 0.65- 0.62 195 164932.33 10.98 71.79 0.62- 0.58 198 166220.69 10.91 68.69 ------------------------------------------------------------------------------------ 4.82- 0.58 1953 395364.93 23.94 81.31 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 195 759153.11 54.79 96.41 4.82- 1.09 390 793744.04 49.13 92.82 4.82- 0.96 585 657473.94 41.22 89.23 4.82- 0.85 780 597341.85 36.77 87.82 4.82- 0.80 975 567832.76 34.27 88.00 4.82- 0.73 1170 515914.75 31.11 84.87 4.82- 0.70 1365 471478.20 28.55 83.22 4.82- 0.65 1560 453252.69 27.21 84.10 4.82- 0.62 1755 421217.10 25.41 82.74 4.82- 0.58 1953 395364.93 23.94 81.31 ------------------------------------------------------------------------------------ 4.82- 0.58 1953 395364.93 23.94 81.31 Scale applied to data: s=0.167624 (maximum obs:5965739.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.028; Rsigma 0.027: data 1953 -> merged 110 With outlier rejection... Rint 0.024; Rsigma 0.027: data 1944 -> merged 110 Rejected total: 9, method kkm 8, method Blessing 1 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585899, 4.831450 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.91 - 1.71 10 10 10.50 100.00 105 1.61 - 1.21 10 10 17.60 100.00 176 1.17 - 1.01 10 10 22.80 100.00 228 0.99 - 0.89 10 10 22.40 100.00 224 0.88 - 0.81 10 10 21.80 100.00 218 0.81 - 0.74 10 10 19.10 100.00 191 0.73 - 0.71 10 10 21.10 100.00 211 0.70 - 0.66 10 10 17.80 100.00 178 0.66 - 0.64 10 10 15.70 100.00 157 0.63 - 0.60 10 10 15.80 100.00 158 --------------------------------------------------------------- 5.91 - 0.60 100 100 18.46 100.00 1846 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:38:31 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.914936 5.917667 5.916898 60.0372 90.0459 60.0146 1805 Reflections read from file xs1714a.hkl; mean (I/sigma) = 26.78 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 888 956 896 909 1370 1212 1220 1805 N (int>3sigma) = 0 756 956 764 764 1238 1046 1038 1539 Mean intensity = 0.0 58.4 28.8 57.9 65.4 47.9 69.4 65.7 66.3 Mean int/sigma = 0.0 25.4 22.6 25.0 26.3 24.3 27.9 27.0 26.8 Lattice type: P chosen Volume: 146.50 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Unitcell: 5.915 5.916 5.917 119.99 90.05 119.94 Niggli form: a.a = 34.986 b.b = 34.997 c.c = 35.010 b.c = -17.494 a.c = -0.028 a.b = -17.465 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.192 [ 1652] Vol = 586.0 Cell: 8.363 8.372 8.370 89.97 89.98 90.02 Volume: 586.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.160 [ 1385] Vol = 439.5 Cell: 5.916 5.915 14.495 89.98 90.03 119.94 Volume: 439.51 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.158 [ 417] Vol = 439.5 Trigonal Cell: 5.916 5.915 14.495 89.98 90.03 119.94 Volume: 439.51 Matrix:-1.0000 1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.047 TETRAGONAL I-lattice R(int) = 0.164 [ 1413] Vol = 293.0 Cell: 5.921 5.918 8.363 89.97 90.00 90.02 Volume: 293.01 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.040 TETRAGONAL I-lattice R(int) = 0.164 [ 1413] Vol = 293.0 Cell: 5.921 5.918 8.363 89.97 90.00 90.02 Volume: 293.01 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.162 [ 1366] Vol = 293.0 Cell: 5.921 8.363 5.918 89.97 89.98 90.00 Volume: 293.01 Matrix: 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.127 [ 1114] Vol = 293.0 Cell: 8.363 5.921 5.918 90.02 90.03 90.00 Volume: 293.01 Matrix:-1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC C-lattice R(int) = 0.143 [ 1146] Vol = 293.0 Cell: 8.363 8.372 5.915 89.97 134.97 90.02 Volume: 293.01 Matrix:-1.0000 0.0000 -1.0000 -1.0000 2.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.119 [ 698] Vol = 146.5 Cell: 5.915 5.916 5.917 119.99 90.05 119.94 Volume: 146.50 Matrix: 1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 956 0 1212 1222 1805 N (int>3sigma) = 0 0 0 0 956 0 1046 1045 1539 Mean intensity = 0.0 0.0 0.0 0.0 28.8 0.0 69.4 64.8 66.3 Mean int/sigma = 0.0 0.0 0.0 0.0 22.6 0.0 27.9 26.5 26.8 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.145 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 19 19 131 412 N I>3s 17 17 72 412 0.8 0.8 0.7 33.8 5.6 5.6 3.7 27.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.191 1540 Fd-3m 1 1 227 C N N N N 37 2284 0.193 1578 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363018 8.372047 8.369721 89.9709 89.9810 90.0180 ZERR 1.00 0.000327 0.004162 0.001876 0.0025 0.0019 0.0137 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4783660- 597693 439 433 27 16.0 1325559.09 56.15 0.021 0.025 569090- 135246 570 569 27 21.1 238915.79 25.96 0.029 0.034 118813- 40584 485 485 27 18.0 88260.90 11.03 0.040 0.051 11404- 1955 459 457 29 15.8 3911.06 2.81 0.147 0.188 ------------------------------------------------------------------------------------------- 4783660- 1955 1953 1944 110 17.7 388119.37 23.52 0.024 0.028 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 476 468 27 17.3 684532.49 43.70 0.022 0.025 0.015 1.01-0.78 566 565 27 20.9 390779.24 22.20 0.019 0.023 0.028 0.78-0.65 560 560 29 19.3 265097.18 15.21 0.028 0.033 0.040 0.65-0.59 351 351 27 13.0 184895.05 11.98 0.042 0.044 0.055 ------------------------------------------------------------------------------------------------------ inf-0.59 1953 1944 110 17.7 388119.37 23.52 0.024 0.028 0.027 inf-0.60 1853 1844 99 18.6 402182.02 24.26 0.024 0.027 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 468 27 27 100.0 17.3 684532.49 191.83 0.022 0.004 1.01-0.78 565 27 27 100.0 20.9 390779.24 106.37 0.019 0.006 0.78-0.65 560 29 29 100.0 19.3 265097.18 70.53 0.028 0.010 0.65-0.59 351 27 27 100.0 13.0 184895.05 50.17 0.042 0.017 -------------------------------------------------------------------------------------------- inf-0.59 1944 110 110 100.0 17.7 388119.37 106.47 0.024 0.007 inf-0.60 1844 99 99 100.0 18.6 402182.02 110.21 0.024 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:45:26 2018) ID: 2932; threads 39; handles 876; mem 518152.00 (1237700.00)kB; time: 1w 4d 23h 50m 56s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.0,peak PF: 697.1, WS: 297.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:228.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.8,peak PF: 697.1, WS: 299.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:45:26 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000015 0.000013 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000017 0.000015 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000012 0.000011 0.000011 ) 5.91502 ( 0.00088 ) 5.91640 ( 0.00088 ) 5.92265 ( 0.00068 ) 60.05206 ( 0.01374 ) 89.98756 ( 0.01061 ) 60.01743 ( 0.01551 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:45:26 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000015 0.000013 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000017 0.000015 0.000015 ) 0.109112 -0.153091 0.115835 ( 0.000012 0.000011 0.000011 ) M - matrix: 0.021570 -0.014368 0.007194 ( 0.000004 0.000003 0.000003 ) -0.014368 0.028712 -0.014353 ( 0.000003 0.000004 0.000003 ) 0.007194 -0.014353 0.021546 ( 0.000003 0.000003 0.000003 ) unit cell: 5.9150(9) 5.9164(9) 5.9227(7) 60.052(14) 89.988(11) 60.017(16) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb PROFFITPEAK info: 639 peaks in the peak location table UB fit with 283 obs out of 302 (total:302,skipped:0) (93.71%) UB - matrix: -0.069830 0.031242 0.089077 ( 0.000054 0.000149 0.000088 ) -0.068691 -0.065614 -0.010114 ( 0.000065 0.000177 0.000104 ) 0.108982 -0.153032 0.116461 ( 0.000062 0.000169 0.000100 ) M - matrix: 0.021472 -0.014352 0.007167 ( 0.000018 0.000027 0.000017 ) -0.014352 0.028700 -0.014376 ( 0.000027 0.000057 0.000029 ) 0.007167 -0.014376 0.021600 ( 0.000017 0.000029 0.000028 ) unit cell: 5.933(7) 5.927(7) 5.911(5) 59.98(11) 89.91(8) 59.91(13) V = 146.8(2) UB fit with 283 obs out of 302 (total:302,skipped:0) (93.71%) UB - matrix: -0.069830 0.031242 0.089077 ( 0.000054 0.000149 0.000088 ) -0.068691 -0.065614 -0.010114 ( 0.000065 0.000177 0.000104 ) 0.108982 -0.153032 0.116461 ( 0.000062 0.000169 0.000100 ) M - matrix: 0.021472 -0.014352 0.007167 ( 0.000018 0.000027 0.000017 ) -0.014352 0.028700 -0.014376 ( 0.000027 0.000057 0.000029 ) 0.007167 -0.014376 0.021600 ( 0.000017 0.000029 0.000028 ) unit cell: 5.933(7) 5.927(7) 5.911(5) 59.98(11) 89.91(8) 59.91(13) V = 146.8(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.069863 0.031232 0.089012 ( 0.000052 0.000143 0.000085 ) -0.068700 -0.065559 -0.010069 ( 0.000061 0.000168 0.000099 ) 0.108735 -0.153003 0.116375 ( 0.000067 0.000183 0.000108 ) M - matrix: 0.021424 -0.014315 0.007127 ( 0.000018 0.000027 0.000017 ) -0.014315 0.028683 -0.014366 ( 0.000027 0.000061 0.000031 ) 0.007127 -0.014366 0.021568 ( 0.000017 0.000031 0.000029 ) UB fit with 280 obs out of 302 (total:302,skipped:0) (92.72%) unit cell: 5.936(7) 5.928(7) 5.916(5) 59.91(11) 89.83(8) 59.92(13) V = 147.1(2) UB fit with 280 obs out of 302 (total:302,skipped:0) (92.72%) UB - matrix: -0.069866 0.031236 0.089035 ( 0.000051 0.000140 0.000084 ) -0.068700 -0.065560 -0.010072 ( 0.000061 0.000168 0.000100 ) 0.108731 -0.152999 0.116403 ( 0.000066 0.000182 0.000109 ) M - matrix: 0.021423 -0.014314 0.007128 ( 0.000018 0.000027 0.000017 ) -0.014314 0.028682 -0.014368 ( 0.000027 0.000061 0.000031 ) 0.007128 -0.014368 0.021579 ( 0.000017 0.000031 0.000029 ) unit cell: 5.936(7) 5.928(7) 5.915(5) 59.92(11) 89.83(8) 59.92(13) V = 147.0(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.069834 0.031220 0.089046 ( 0.000051 0.000140 0.000084 ) -0.068688 -0.065561 -0.010041 ( 0.000061 0.000168 0.000100 ) 0.108723 -0.152996 0.116403 ( 0.000066 0.000182 0.000108 ) M - matrix: 0.021416 -0.014311 0.007127 ( 0.000018 0.000027 0.000017 ) -0.014311 0.028681 -0.014371 ( 0.000027 0.000060 0.000031 ) 0.007127 -0.014371 0.021580 ( 0.000017 0.000031 0.000029 ) UB fit with 280 obs out of 302 (total:302,skipped:0) (92.72%) unit cell: 5.937(7) 5.929(7) 5.915(5) 59.91(11) 89.82(8) 59.92(13) V = 147.1(2) 302 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Run 4 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069834 0.031220 0.089046 ( 0.000051 0.000140 0.000084 ) -0.068688 -0.065561 -0.010041 ( 0.000061 0.000168 0.000100 ) 0.108723 -0.152996 0.116403 ( 0.000066 0.000182 0.000108 ) M - matrix: 0.021416 -0.014311 0.007127 ( 0.000018 0.000027 0.000017 ) -0.014311 0.028681 -0.014371 ( 0.000027 0.000060 0.000031 ) 0.007127 -0.014371 0.021580 ( 0.000017 0.000031 0.000029 ) UB fit with 280 obs out of 302 (total:302,skipped:0) (92.72%) unit cell: 5.937(7) 5.929(7) 5.915(5) 59.91(11) 89.82(8) 59.92(13) V = 147.1(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 277 obs out of 302 (total:302,skipped:0) (91.72%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb 4 of 218 peaks identified as outliers and rejected 214 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 214 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 214 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 1.48 | 21 | 1.054 ( 0.196) | 1.224 ( 0.599) | 1.428 ( 1.088) | 1.41- 1.15 | 21 | 1.053 ( 0.069) | 1.173 ( 0.294) | 1.324 ( 0.741) | 1.15- 0.98 | 21 | 1.024 ( 0.098) | 1.030 ( 0.126) | 0.991 ( 0.317) | 0.97- 0.89 | 21 | 1.033 ( 0.086) | 1.033 ( 0.127) | 1.180 ( 0.443) | 0.89- 0.82 | 21 | 1.035 ( 0.081) | 1.017 ( 0.107) | 1.207 ( 0.581) | 0.81- 0.76 | 21 | 1.019 ( 0.091) | 0.983 ( 0.130) | 1.045 ( 0.432) | 0.75- 0.71 | 21 | 1.031 ( 0.027) | 0.962 ( 0.110) | 1.228 ( 0.519) | 0.71- 0.67 | 21 | 1.000 ( 0.040) | 0.877 ( 0.040) | 1.362 ( 0.536) | 0.67- 0.64 | 21 | 0.961 ( 0.030) | 0.835 ( 0.041) | 1.237 ( 0.472) | 0.63- 0.59 | 25 | 0.925 ( 0.037) | 0.797 ( 0.035) | 1.229 ( 0.440) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 0.59 | 214 | 1.012 ( 0.098) | 0.989 ( 0.261) | 1.223 ( 0.604) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) UB - matrix: -0.070080 0.031398 0.088717 ( 0.000019 0.000053 0.000034 ) -0.068794 -0.065771 -0.010257 ( 0.000024 0.000068 0.000044 ) 0.108867 -0.152851 0.116178 ( 0.000016 0.000045 0.000029 ) M - matrix: 0.021496 -0.014316 0.007136 ( 0.000005 0.000008 0.000006 ) -0.014316 0.028675 -0.014298 ( 0.000008 0.000017 0.000009 ) 0.007136 -0.014298 0.021473 ( 0.000006 0.000009 0.000009 ) unit cell: 5.921(3) 5.917(3) 5.9223(19) 60.06(4) 89.99(3) 60.02(5) V = 146.89(9) OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 OTKP changes: 214 1 1 1 UB - matrix: -0.069908 0.031361 0.088770 ( 0.000018 0.000051 0.000033 ) -0.068735 -0.065797 -0.010074 ( 0.000023 0.000064 0.000042 ) 0.108888 -0.152865 0.116217 ( 0.000016 0.000045 0.000029 ) M - matrix: 0.021468 -0.014315 0.007141 ( 0.000005 0.000008 0.000005 ) -0.014315 0.028680 -0.014319 ( 0.000008 0.000017 0.000009 ) 0.007141 -0.014319 0.021488 ( 0.000005 0.000009 0.000009 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.927(3) 5.920(3) 5.9233(18) 60.02(4) 89.98(3) 60.01(5) V = 147.03(9) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069908 0.031361 0.088770 ( 0.000018 0.000051 0.000033 ) -0.068735 -0.065797 -0.010074 ( 0.000023 0.000064 0.000042 ) 0.108888 -0.152865 0.116217 ( 0.000016 0.000045 0.000029 ) M - matrix: 0.021468 -0.014315 0.007141 ( 0.000005 0.000008 0.000005 ) -0.014315 0.028680 -0.014319 ( 0.000008 0.000017 0.000009 ) 0.007141 -0.014319 0.021488 ( 0.000005 0.000009 0.000009 ) UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) unit cell: 5.927(3) 5.920(3) 5.9233(18) 60.02(4) 89.98(3) 60.01(5) V = 147.03(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 214 obs out of 214 (total:214,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb 3 of 219 peaks identified as outliers and rejected 216 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 216 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 216 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 1.41 | 22 | 1.052 ( 0.185) | 1.216 ( 0.589) | 1.334 ( 0.982) | 1.41- 1.12 | 22 | 1.058 ( 0.073) | 1.152 ( 0.324) | 1.283 ( 0.647) | 1.12- 0.97 | 22 | 1.022 ( 0.097) | 1.041 ( 0.127) | 1.008 ( 0.365) | 0.97- 0.85 | 22 | 1.023 ( 0.100) | 1.033 ( 0.132) | 1.109 ( 0.448) | 0.85- 0.81 | 22 | 1.060 ( 0.064) | 1.028 ( 0.110) | 1.225 ( 0.556) | 0.81- 0.73 | 22 | 1.004 ( 0.073) | 0.952 ( 0.110) | 1.194 ( 0.501) | 0.73- 0.69 | 22 | 1.017 ( 0.036) | 0.930 ( 0.091) | 1.375 ( 0.596) | 0.69- 0.66 | 22 | 0.981 ( 0.041) | 0.857 ( 0.047) | 1.152 ( 0.423) | 0.65- 0.62 | 22 | 0.948 ( 0.045) | 0.828 ( 0.037) | 1.166 ( 0.448) | 0.62- 0.59 | 18 | 0.931 ( 0.039) | 0.786 ( 0.030) | 1.290 ( 0.429) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 0.59 | 216 | 1.011 ( 0.096) | 0.986 ( 0.265) | 1.212 ( 0.577) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 154 | 1.120 ( 0.124) | 1.253 ( 0.482) | 1.178 ( 0.626) | 13.3-19.0 | 154 | 1.080 ( 0.054) | 1.130 ( 0.259) | 1.248 ( 0.545) | 19.0-23.2 | 154 | 1.071 ( 0.075) | 1.141 ( 0.366) | 1.172 ( 0.498) | 23.2-27.2 | 155 | 1.037 ( 0.082) | 1.082 ( 0.301) | 1.215 ( 0.593) | 27.2-30.9 | 154 | 1.012 ( 0.078) | 0.999 ( 0.176) | 1.213 ( 0.512) | 30.9-33.7 | 154 | 0.986 ( 0.085) | 0.925 ( 0.100) | 1.186 ( 0.516) | 33.7-36.9 | 154 | 0.966 ( 0.079) | 0.902 ( 0.099) | 1.187 ( 0.492) | 36.9-39.7 | 154 | 0.950 ( 0.094) | 0.878 ( 0.149) | 1.175 ( 0.532) | 39.7-42.8 | 154 | 0.924 ( 0.085) | 0.836 ( 0.087) | 1.184 ( 0.518) | 42.8-49.9 | 156 | 0.937 ( 0.082) | 0.818 ( 0.067) | 1.158 ( 0.448) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1543 | 1.008 ( 0.106) | 0.996 ( 0.284) | 1.192 ( 0.531) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0012 b=1.04 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3682287 PROFFITPEAK - Finished at Tue Mar 27 14:45:41 2018 PROFFITMAIN - Started at Tue Mar 27 14:45:41 2018 OTKP changes: 1543 2 3 4 OTKP changes: 1543 2 3 4 UB - matrix: -0.070199 0.031083 0.088919 ( 0.000013 0.000013 0.000012 ) -0.068736 -0.065877 -0.010485 ( 0.000013 0.000013 0.000013 ) 0.109163 -0.153035 0.116318 ( 0.000011 0.000011 0.000010 ) M - matrix: 0.021569 -0.014360 0.007176 ( 0.000003 0.000003 0.000002 ) -0.014360 0.028726 -0.014346 ( 0.000003 0.000004 0.000002 ) 0.007176 -0.014346 0.021546 ( 0.000002 0.000002 0.000003 ) UB fit with 1543 obs out of 1543 (total:1543,skipped:0) (100.00%) unit cell: 5.9127(7) 5.9135(7) 5.9146(6) 60.044(12) 90.019(9) 60.023(13) V = 146.35(3) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070045 0.030661 0.088968 ( 0.000029 0.000028 0.000016 ) -0.068248 -0.066140 -0.010497 ( 0.000025 0.000025 0.000015 ) 0.109067 -0.153052 0.115965 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021460 -0.014327 0.007133 ( 0.000008 0.000006 0.000004 ) -0.014327 0.028740 -0.014327 ( 0.000006 0.000008 0.000005 ) 0.007133 -0.014327 0.021473 ( 0.000004 0.000005 0.000004 ) unit cell: 5.9277(14) 5.9137(14) 5.9249(11) 60.02(2) 89.963(18) 60.00(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070318 0.030928 0.088797 ( 0.000026 0.000026 0.000015 ) -0.068410 -0.066117 -0.010696 ( 0.000024 0.000023 0.000013 ) 0.109322 -0.153276 0.116358 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021576 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028822 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014382 0.021539 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9078(13) 5.9186(10) 60.05(2) 90.075(16) 60.00(2) V = 146.30(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.801) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070318 0.030928 0.088797 ( 0.000026 0.000026 0.000015 ) -0.068410 -0.066117 -0.010696 ( 0.000024 0.000023 0.000013 ) 0.109322 -0.153276 0.116358 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021576 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028822 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014382 0.021539 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9078(13) 5.9186(10) 60.05(2) 90.075(16) 60.00(2) V = 146.30(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070318 0.030928 0.088797 ( 0.000026 0.000026 0.000015 ) -0.068410 -0.066117 -0.010696 ( 0.000024 0.000023 0.000013 ) 0.109322 -0.153276 0.116358 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021576 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028822 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014382 0.021539 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9164(13) 5.9078(13) 5.9186(10) 60.05(2) 90.075(16) 60.00(2) V = 146.30(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031354 0.088639 ( 0.000026 0.000022 0.000028 ) -0.068575 -0.066007 -0.010228 ( 0.000031 0.000027 0.000033 ) 0.108987 -0.152634 0.116244 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021538 -0.014316 0.007130 ( 0.000007 0.000005 0.000005 ) -0.014316 0.028637 -0.014288 ( 0.000005 0.000007 0.000005 ) 0.007130 -0.014288 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(17) 5.9211(16) 5.9222(13) 60.03(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070352 0.031192 0.088840 ( 0.000023 0.000020 0.000025 ) -0.068773 -0.065861 -0.010343 ( 0.000030 0.000026 0.000032 ) 0.109160 -0.153142 0.116567 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021595 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028763 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014399 0.021587 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9100(16) 5.9169(16) 5.9151(12) 59.94(2) 89.944(19) 60.01(3) V = 146.21(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.801) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070352 0.031192 0.088840 ( 0.000023 0.000020 0.000025 ) -0.068773 -0.065861 -0.010343 ( 0.000030 0.000026 0.000032 ) 0.109160 -0.153142 0.116567 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021595 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028763 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014399 0.021587 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9100(16) 5.9169(16) 5.9151(12) 59.94(2) 89.944(19) 60.01(3) V = 146.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070352 0.031192 0.088840 ( 0.000023 0.000020 0.000025 ) -0.068773 -0.065861 -0.010343 ( 0.000030 0.000026 0.000032 ) 0.109160 -0.153142 0.116567 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021595 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028763 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014399 0.021587 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9100(16) 5.9169(16) 5.9151(12) 59.94(2) 89.944(19) 60.01(3) V = 146.21(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) UB - matrix: -0.070173 0.031434 0.088669 ( 0.000019 0.000054 0.000035 ) -0.068822 -0.065790 -0.010343 ( 0.000025 0.000071 0.000046 ) 0.108889 -0.152841 0.116167 ( 0.000016 0.000044 0.000028 ) M - matrix: 0.021518 -0.014321 0.007139 ( 0.000006 0.000008 0.000006 ) -0.014321 0.028677 -0.014287 ( 0.000008 0.000017 0.000009 ) 0.007139 -0.014287 0.021464 ( 0.000006 0.000009 0.000009 ) unit cell: 5.918(3) 5.914(3) 5.9220(19) 60.08(4) 90.02(3) 60.03(5) V = 146.79(10) OTKP changes: 216 1 1 1 OTKP changes: 216 1 1 1 OTKP changes: 216 1 1 1 UB - matrix: -0.070107 0.031405 0.088942 ( 0.000018 0.000051 0.000033 ) -0.068682 -0.066146 -0.010059 ( 0.000023 0.000065 0.000042 ) 0.109195 -0.153113 0.116536 ( 0.000015 0.000042 0.000027 ) M - matrix: 0.021556 -0.014378 0.007181 ( 0.000005 0.000008 0.000005 ) -0.014378 0.028805 -0.014385 ( 0.000008 0.000016 0.000008 ) 0.007181 -0.014385 0.021592 ( 0.000005 0.000008 0.000009 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.915(3) 5.907(3) 5.9090(18) 60.03(4) 90.00(3) 60.01(5) V = 146.07(9) Run 4 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.801) HKL list info: 418 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070107 0.031405 0.088942 ( 0.000018 0.000051 0.000033 ) -0.068682 -0.066146 -0.010059 ( 0.000023 0.000065 0.000042 ) 0.109195 -0.153113 0.116536 ( 0.000015 0.000042 0.000027 ) M - matrix: 0.021556 -0.014378 0.007181 ( 0.000005 0.000008 0.000005 ) -0.014378 0.028805 -0.014385 ( 0.000008 0.000016 0.000008 ) 0.007181 -0.014385 0.021592 ( 0.000005 0.000008 0.000009 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.915(3) 5.907(3) 5.9090(18) 60.03(4) 90.00(3) 60.01(5) V = 146.07(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070107 0.031405 0.088942 ( 0.000018 0.000051 0.000033 ) -0.068682 -0.066146 -0.010059 ( 0.000023 0.000065 0.000042 ) 0.109195 -0.153113 0.116536 ( 0.000015 0.000042 0.000027 ) M - matrix: 0.021556 -0.014378 0.007181 ( 0.000005 0.000008 0.000005 ) -0.014378 0.028805 -0.014385 ( 0.000008 0.000016 0.000008 ) 0.007181 -0.014385 0.021592 ( 0.000005 0.000008 0.000009 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 5.915(3) 5.907(3) 5.9090(18) 60.03(4) 90.00(3) 60.01(5) V = 146.07(9) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070116 0.031056 0.088862 ( 0.000013 0.000013 0.000012 ) -0.068712 -0.065777 -0.010536 ( 0.000015 0.000015 0.000014 ) 0.109187 -0.153055 0.116380 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021559 -0.014369 0.007200 ( 0.000004 0.000003 0.000002 ) -0.014369 0.028717 -0.014360 ( 0.000003 0.000004 0.000002 ) 0.007200 -0.014360 0.021552 ( 0.000002 0.000002 0.000003 ) UB fit with 1543 obs out of 1543 (total:1543,skipped:0) (100.00%) unit cell: 5.9172(8) 5.9179(8) 5.9168(6) 60.038(13) 90.060(10) 60.013(15) V = 146.54(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 57 reflections under beam stop or inside a detector rejection region 13 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof 2106 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:45:45 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.801) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.801) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.801) PROFFIT INFO: signal sum: min=249.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2944386.2611 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4711018.0000 PROFFIT INFO: sig(Inet): min=96.4398 max=47445.8711 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.10 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 12 74 193 427 474 820 1381 1918 2106 Percent 0.0 0.0 0.6 3.5 9.2 20.3 22.5 38.9 65.6 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2106 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2106 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711018- 1222576 210 1957869.44 123.58 100.00 1218365- 713385 210 928543.24 106.94 100.00 712280- 280684 210 462169.80 97.46 100.00 279976- 179865 210 215735.21 74.12 100.00 179820- 135852 210 158187.47 51.91 100.00 135167- 102323 210 116620.04 37.62 100.00 102300- 77994 210 90098.59 30.35 100.00 77925- 6001 210 45205.19 20.58 100.00 5943- 3230 210 4326.86 5.59 98.10 3228- 924 216 2420.02 4.17 67.59 ------------------------------------------------------------------------------------ 4711018- 924 2106 396990.24 55.09 96.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 210 693714.09 86.64 99.05 1.41- 1.07 210 606272.38 69.40 98.57 1.07- 0.96 210 454529.47 62.49 97.14 0.96- 0.83 210 438988.66 56.71 96.19 0.83- 0.75 210 407131.55 58.46 96.67 0.75- 0.70 210 317669.61 49.16 96.67 0.70- 0.63 210 304311.22 48.49 97.14 0.63- 0.58 210 290888.67 45.62 95.24 0.58- 0.52 210 253938.39 39.95 92.86 0.52- 0.40 216 207862.02 34.54 95.37 ------------------------------------------------------------------------------------ 5.26- 0.40 2106 396990.24 55.09 96.49 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:45:45 2018 Sorting 2106 observations 242 unique observations with > 7.00 F2/sig(F2) 2106 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 0 48 363 Total number of frames 363 Maximum number of 242 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2106 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 24 184 Total number of frames 184 1699 observations > 7.00 F2/sig(F2) 1699 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 24 184 Total number of frames 184 Removing 'redundancy=1' reflections Average redundancy: 7.0 (Out of 1699 removed 53 = 1646, unique = 234) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1646 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 24 184 Total number of frames 184 234 unique data precomputed (should be 234) 234 unique data with 1646 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.0 (Out of 1646 removed 0 = 1646, unique = 234) 234 unique data precomputed (should be 234) 234 unique data with 1646 observations RMS deviation of equivalent data = 0.71572 Rint = 0.68575 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66635, wR= 3.90996 Trying model 1 (ne=2, no=0)... Results: Rint= 0.74773, wR= 2.92531, Acormin=-0.041, Acormax=2.068, Acor_av=0.613 F test: Probability=0.000, F= 0.791 Trying model 2 (ne=2, no=1)... Results: Rint= 0.91708, wR= 2.76490, Acormin=-0.467, Acormax=1.919, Acor_av=0.341 F test: Probability=0.000, F= 0.525 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75916, wR= 2.29737, Acormin=-0.144, Acormax=2.316, Acor_av=0.487 F test: Probability=0.000, F= 0.763 Trying model 4 (ne=4, no=1)... Results: Rint= 0.90904, wR= 2.33729, Acormin=-0.485, Acormax=2.103, Acor_av=0.265 F test: Probability=0.000, F= 0.531 Trying model 5 (ne=4, no=3)... Results: Rint= 0.97243, wR= 2.04200, Acormin=-1.254, Acormax=1.539, Acor_av=0.094 F test: Probability=0.000, F= 0.462 Trying model 6 (ne=6, no=0)... Results: Rint= 0.79592, wR= 2.38068, Acormin=-0.241, Acormax=2.844, Acor_av=0.420 F test: Probability=0.000, F= 0.687 Trying model 7 (ne=6, no=1)... Results: Rint= 0.94287, wR= 2.39504, Acormin=-0.643, Acormax=2.282, Acor_av=0.199 F test: Probability=0.000, F= 0.489 Trying model 8 (ne=6, no=3)... Results: Rint= 0.98679, wR= 2.38946, Acormin=-1.244, Acormax=1.593, Acor_av=0.068 F test: Probability=0.000, F= 0.444 Trying model 9 (ne=6, no=5)... Results: Rint= 1.03912, wR= 2.18192, Acormin=-0.718, Acormax=3.406, Acor_av=0.031 F test: Probability=0.000, F= 0.397 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86920, wR= 2.06510, Acormin=-0.610, Acormax=3.068, Acor_av=0.325 F test: Probability=0.000, F= 0.569 Trying model 11 (ne=8, no=1)... Results: Rint= 1.01552, wR= 1.84992, Acormin=-1.200, Acormax=1.392, Acor_av=0.043 F test: Probability=0.000, F= 0.416 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98504, wR= 1.40171, Acormin=-0.040, Acormax=0.078, Acor_av=0.002 F test: Probability=0.000, F= 0.440 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99036, wR= 1.43844, Acormin=-0.041, Acormax=0.086, Acor_av=0.002 F test: Probability=0.000, F= 0.432 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00419, wR= 1.36630, Acormin=-0.041, Acormax=0.139, Acor_av=0.001 F test: Probability=0.000, F= 0.415 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.85384 There are 184 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 188 pars with 17766 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71572 Using Levenberg-Marquardt: 0.00010 New wR= 0.69481 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68575 with corrections 0.65332 Rint for all data: 0.85384 with corrections 0.83150 9 observations identified as outliers and rejected Cycle 2 wR= 0.67166 Using Levenberg-Marquardt: 0.00001 New wR= 0.70376 Using Levenberg-Marquardt: 0.00010 New wR= 0.69742 Using Levenberg-Marquardt: 0.00100 New wR= 0.67565 Using Levenberg-Marquardt: 0.01000 New wR= 0.66721 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66635 with corrections 0.64126 Rint for all data: 0.85384 with corrections 0.83687 11 observations identified as outliers and rejected Cycle 3 wR= 0.64049 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63914 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65303 with corrections 0.63134 Rint for all data: 0.85384 with corrections 0.83978 6 observations identified as outliers and rejected Cycle 4 wR= 0.63154 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63232 Using Levenberg-Marquardt: 0.10000 New wR= 0.62953 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64751 with corrections 0.62739 Rint for all data: 0.85384 with corrections 0.84020 8 observations identified as outliers and rejected Cycle 5 wR= 0.61161 Using Levenberg-Marquardt: 0.01000 New wR= 0.83210 Using Levenberg-Marquardt: 0.10000 New wR= 0.61009 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64191 with corrections 0.62257 Rint for all data: 0.85384 with corrections 0.83975 7 observations identified as outliers and rejected Final wR= 0.61009 Final frame scales: Min= 0.6386 Max= 2.4337 Final absorption correction factors: Amin= 0.3603 Amax= 1.3376 PROFFIT INFO: Inet (after scale3 abspack): min=768.0205 max=5325750.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=111.7498 max=64918.6875 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2106 reflections read from tmp file 1636 reflections are rejected (1541 as outliers, 95 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 84 45 18 9 3 2 1 0 1 Initial Chi^2= 0.83722 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.42823 Current error model SIG(F2)^2 = 551.02*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 235.96*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 235.96*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5325751- 1197122 210 1922822.98 95.78 100.00 1185015- 678803 210 896975.43 48.27 100.00 678465- 267156 210 438912.95 43.58 100.00 266590- 172542 210 209104.25 32.62 100.00 171786- 132985 210 151268.94 22.34 100.00 132610- 101925 210 118658.30 17.58 100.00 101725- 73230 210 86670.55 13.68 100.00 73058- 6249 210 42787.40 9.81 95.24 6246- 3129 210 4230.40 3.40 51.90 3122- 768 216 2280.00 2.93 32.87 ------------------------------------------------------------------------------------ 5325751- 768 2106 386273.99 28.92 87.84 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 210 726878.01 62.08 98.10 1.41- 1.07 210 595808.48 43.88 94.76 1.07- 0.96 210 474652.56 32.60 92.38 0.96- 0.83 210 426114.67 28.57 84.76 0.83- 0.75 210 391562.72 27.18 86.19 0.75- 0.70 210 304792.81 21.75 86.19 0.70- 0.63 210 277812.41 21.09 83.33 0.63- 0.58 210 282582.79 19.83 86.19 0.58- 0.52 210 219664.57 17.47 82.38 0.52- 0.40 216 169076.55 15.18 84.26 ------------------------------------------------------------------------------------ 5.26- 0.40 2106 386273.99 28.92 87.84 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 210 726878.01 62.08 98.10 5.26- 1.07 420 661343.24 52.98 96.43 5.26- 0.96 630 599113.01 46.19 95.08 5.26- 0.83 840 555863.43 41.78 92.50 5.26- 0.75 1050 523003.29 38.86 91.24 5.26- 0.70 1260 486634.87 36.01 90.40 5.26- 0.63 1470 456803.09 33.88 89.39 5.26- 0.58 1680 435025.56 32.12 88.99 5.26- 0.52 1890 411096.56 30.50 88.25 5.26- 0.40 2106 386273.99 28.92 87.84 ------------------------------------------------------------------------------------ 5.26- 0.40 2106 386273.99 28.92 87.84 Scale applied to data: s=0.187767 (maximum obs:5325750.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.840; Rsigma 0.023: data 2106 -> merged 307 With outlier rejection... Rint 0.748; Rsigma 0.023: data 1960 -> merged 307 Rejected total: 146, method kkm 133, method Blessing 13 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404354, 5.272127 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 10.07 100.00 151 1.46 - 1.12 15 15 15.93 100.00 239 1.08 - 0.96 15 15 13.47 100.00 202 0.96 - 0.86 15 15 12.27 100.00 184 0.86 - 0.79 15 15 10.67 100.00 160 0.79 - 0.73 15 15 9.47 100.00 142 0.73 - 0.69 15 15 8.07 100.00 121 0.69 - 0.65 15 15 8.27 100.00 124 0.65 - 0.63 15 15 5.33 100.00 80 0.63 - 0.60 21 21 5.24 100.00 110 --------------------------------------------------------------- 5.92 - 0.60 156 156 9.70 100.00 1513 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:45:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917173 5.917888 5.916754 60.0377 90.0596 60.0132 1959 Reflections read from file xs1714a.hkl; mean (I/sigma) = 27.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 963 1049 968 983 1490 1311 1319 1959 N (int>3sigma) = 0 845 1049 850 859 1372 1154 1147 1714 Mean intensity = 0.0 57.8 29.4 57.3 64.8 47.6 69.6 67.1 67.1 Mean int/sigma = 0.0 26.3 23.8 25.7 27.2 25.2 29.0 28.4 28.0 Lattice type: P chosen Volume: 146.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 Unitcell: 5.915 5.917 5.917 90.06 119.95 119.97 Niggli form: a.a = 34.992 b.b = 35.008 c.c = 35.013 b.c = -0.036 a.c = -17.475 a.b = -17.484 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.060 CUBIC F-lattice R(int) = 0.176 [ 1806] Vol = 586.2 Cell: 8.372 8.371 8.363 90.02 90.00 90.02 Volume: 586.16 Matrix:-1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.165 [ 1531] Vol = 439.6 Cell: 5.919 5.917 14.500 90.05 90.00 120.03 Volume: 439.62 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.153 [ 481] Vol = 439.6 Trigonal Cell: 5.919 5.917 14.500 90.05 90.00 120.03 Volume: 439.62 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.028 TETRAGONAL I-lattice R(int) = 0.152 [ 1567] Vol = 293.1 Cell: 5.921 5.919 8.363 89.99 89.98 90.01 Volume: 293.08 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.021 TETRAGONAL I-lattice R(int) = 0.152 [ 1567] Vol = 293.1 Cell: 5.919 5.921 8.363 90.02 90.01 90.01 Volume: 293.08 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 1519] Vol = 293.1 Cell: 5.919 5.921 8.363 89.98 89.99 90.01 Volume: 293.08 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.151 [ 1517] Vol = 293.1 Cell: 5.915 8.372 5.918 89.98 89.95 89.99 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.017 MONOCLINIC I-lattice R(int) = 0.147 [ 1209] Vol = 293.1 Cell: 5.921 5.919 8.363 90.01 90.02 90.01 Volume: 293.08 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.034 MONOCLINIC I-lattice R(int) = 0.137 [ 1205] Vol = 293.1 Cell: 5.915 5.918 8.372 90.02 90.01 89.95 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.012 MONOCLINIC I-lattice R(int) = 0.131 [ 1229] Vol = 293.1 Cell: 5.915 8.372 5.918 89.98 90.05 90.01 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.024 MONOCLINIC I-lattice R(int) = 0.135 [ 1208] Vol = 293.1 Cell: 5.918 5.915 8.372 89.99 90.02 90.05 Volume: 293.08 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.050 MONOCLINIC C-lattice R(int) = 0.140 [ 1250] Vol = 293.1 Cell: 10.249 5.917 5.917 90.06 125.23 89.96 Volume: 293.08 Matrix:-2.0000 2.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.115 [ 756] Vol = 146.5 Cell: 5.915 5.917 5.917 90.06 119.95 119.97 Volume: 146.54 Matrix:-1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1049 0 1312 1311 1959 N (int>3sigma) = 0 0 0 0 1049 0 1151 1154 1714 Mean intensity = 0.0 0.0 0.0 0.0 29.4 0.0 67.3 69.6 67.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 27.9 29.0 28.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.130 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 143 448 N I>3s 19 19 90 448 0.8 0.8 0.7 34.3 6.3 6.3 3.9 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.176 1682 Fd-3m 1 1 227 C N N N N 37 2284 0.178 1720 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.372201 8.371245 8.363497 90.0245 89.9959 90.0192 ZERR 1.00 0.001766 0.003921 0.000304 0.0129 0.0018 0.0024 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3089913- 642457 307 283 30 9.4 1008802.91 58.03 0.615 0.555 641364- 501320 256 243 30 8.1 549860.69 38.28 0.883 0.774 498458- 409341 244 230 30 7.7 414096.59 35.93 0.891 0.875 403143- 300560 259 246 30 8.2 314701.28 24.31 0.951 1.046 299152- 218739 235 207 30 6.9 183702.57 18.08 0.820 0.916 217870- 163210 252 225 30 7.5 153173.82 21.87 0.663 0.729 160289- 94130 214 204 30 6.8 106025.75 15.43 0.537 0.516 93615- 72168 137 128 30 4.3 85557.43 13.25 0.470 0.296 71536- 49624 99 92 30 3.1 61817.35 11.16 0.435 0.311 49305- 1565 103 102 37 2.8 24689.86 5.72 0.740 0.765 ------------------------------------------------------------------------------------------- 3089913- 1565 2106 1960 307 6.4 359715.72 28.11 0.748 0.718 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.12 418 391 30 13.0 618219.52 51.63 0.724 0.778 0.014 1.08-0.86 407 387 30 12.9 424338.98 29.80 0.873 0.989 0.022 0.86-0.73 322 306 31 9.9 354776.33 24.94 0.699 0.675 0.027 0.72-0.65 266 246 32 7.7 273031.40 21.29 0.802 0.798 0.030 0.65-0.60 207 181 32 5.7 232683.77 18.40 0.790 0.782 0.034 0.60-0.56 160 144 32 4.5 184890.74 16.25 0.501 0.411 0.039 0.56-0.52 135 123 34 3.6 214287.63 17.96 0.617 0.635 0.038 0.52-0.49 105 97 31 3.1 155475.13 14.16 0.554 0.387 0.043 0.49-0.45 56 55 30 1.8 165010.67 14.93 0.411 0.290 0.042 0.45-0.40 30 30 25 1.2 137281.04 14.04 0.361 0.361 0.045 ------------------------------------------------------------------------------------------------------ inf-0.40 2106 1960 307 6.4 359715.72 28.11 0.748 0.718 0.023 inf-0.60 1624 1514 156 9.7 412233.63 31.68 0.772 0.805 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.12 391 30 30 100.0 13.0 618219.52 207.77 0.724 0.004 1.08-0.86 387 30 30 100.0 12.9 424338.98 128.23 0.873 0.008 0.86-0.73 306 31 31 100.0 9.9 354776.33 93.82 0.699 0.011 0.72-0.65 246 32 32 100.0 7.7 273031.40 73.20 0.802 0.015 0.65-0.60 181 32 32 100.0 5.7 232683.77 56.30 0.790 0.019 0.60-0.56 144 35 32 91.4 4.5 184890.74 41.52 0.501 0.020 0.56-0.52 123 37 34 91.9 3.6 214287.63 44.21 0.617 0.023 0.52-0.49 97 50 31 62.0 3.1 155475.13 31.55 0.554 0.028 0.49-0.45 55 66 30 45.5 1.8 165010.67 23.40 0.411 0.034 0.45-0.40 30 121 25 20.7 1.2 137281.04 16.49 0.361 0.033 -------------------------------------------------------------------------------------------- inf-0.40 1960 464 307 66.2 6.4 359715.72 104.10 0.748 0.013 inf-0.60 1514 156 156 100.0 9.7 412233.63 124.07 0.772 0.010 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 1.0 -1.0 2.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 1.0 -1.0 2.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: 0.079489 0.015528 -0.024900 ( 0.000007 0.000006 0.000007 ) 0.029088 -0.032888 0.072513 ( 0.000009 0.000007 0.000009 ) 0.003597 -0.076527 -0.036256 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007178 0.000002 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007179 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000003 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.079489 0.015528 -0.024900 ( 0.000007 0.000006 0.000007 ) 0.029088 -0.032888 0.072513 ( 0.000009 0.000007 0.000009 ) 0.003597 -0.076527 -0.036256 ( 0.000006 0.000005 0.000006 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3723(7) 8.3713(6) 8.3635(8) 90.025(7) 89.997(7) 90.019(6) V = 586.17(9) unit cell: 8.3690(2) 8.3690(2) 8.3690(2) 90.0 90.0 90.0 V = 586.17(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.801) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.801) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.801) PROFFIT INFO: signal sum: min=249.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2944386.2611 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4711018.0000 PROFFIT INFO: sig(Inet): min=96.4398 max=47445.8711 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=229.10 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 24 148 386 854 948 1640 2762 3836 4212 Percent 0.0 0.0 0.6 3.5 9.2 20.3 22.5 38.9 65.6 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2106 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2106 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4711018- 1222576 210 1957869.44 123.58 100.00 1218365- 713385 210 928543.24 106.94 100.00 712280- 280684 210 462169.80 97.46 100.00 279976- 179865 210 215735.21 74.12 100.00 179820- 135852 210 158187.47 51.91 100.00 135167- 102323 210 116620.04 37.62 100.00 102300- 77994 210 90098.59 30.35 100.00 77925- 6001 210 45205.19 20.58 100.00 5943- 3230 210 4326.86 5.59 98.10 3228- 924 216 2420.02 4.17 67.59 ------------------------------------------------------------------------------------ 4711018- 924 2106 396990.24 55.09 96.49 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 210 746396.85 94.14 100.00 1.39- 1.12 210 793673.15 67.15 100.00 1.12- 0.96 210 397369.79 68.04 98.10 0.96- 0.88 210 402059.34 63.90 96.19 0.85- 0.81 210 484683.12 70.56 99.52 0.81- 0.73 210 268115.70 42.94 99.52 0.73- 0.70 210 190749.91 34.51 86.19 0.70- 0.65 210 344818.03 50.61 97.62 0.65- 0.62 210 178546.27 30.31 90.00 0.62- 0.58 216 169976.37 29.44 97.69 ------------------------------------------------------------------------------------ 4.82- 0.58 2106 396990.24 55.09 96.49 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:45:46 2018 Sorting 2106 observations 84 unique observations with > 7.00 F2/sig(F2) 2106 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 0 48 363 Total number of frames 363 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2106 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 9 74 Total number of frames 74 1699 observations > 7.00 F2/sig(F2) 1699 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 9 74 Total number of frames 74 Removing 'redundancy=1' reflections Average redundancy: 18.2 (Out of 1699 removed 3 = 1696, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1696 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 9 74 Total number of frames 74 93 unique data precomputed (should be 93) 93 unique data with 1696 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 18.2 (Out of 1696 removed 0 = 1696, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 1696 observations RMS deviation of equivalent data = 0.13895 Rint = 0.11105 3 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.11060, wR= 0.13847 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07969, wR= 0.09839, Acormin=0.796, Acormax=1.253, Acor_av=0.990 F test: Probability=1.000, F= 1.920 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07477, wR= 0.09145, Acormin=0.742, Acormax=1.298, Acor_av=0.958 F test: Probability=0.994, F= 1.134 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06470, wR= 0.08348, Acormin=0.728, Acormax=1.294, Acor_av=0.943 F test: Probability=1.000, F= 1.331 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06212, wR= 0.07959, Acormin=0.670, Acormax=1.273, Acor_av=0.888 F test: Probability=0.943, F= 1.083 Trying model 5 (ne=4, no=3)... Results: Rint= 0.05139, wR= 0.06894, Acormin=0.625, Acormax=1.282, Acor_av=0.855 F test: Probability=1.000, F= 1.575 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06223, wR= 0.08129, Acormin=0.738, Acormax=1.301, Acor_av=0.940 F test: Probability=0.000, F= 0.681 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05959, wR= 0.07738, Acormin=0.648, Acormax=1.292, Acor_av=0.877 F test: Probability=0.000, F= 0.741 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04970, wR= 0.06645, Acormin=0.612, Acormax=1.300, Acor_av=0.863 F test: Probability=0.877, F= 1.060 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04307, wR= 0.05853, Acormin=0.493, Acormax=1.222, Acor_av=0.803 F test: Probability=1.000, F= 1.402 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05944, wR= 0.07846, Acormin=0.701, Acormax=1.282, Acor_av=0.910 F test: Probability=0.000, F= 0.526 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05459, wR= 0.07129, Acormin=0.570, Acormax=1.205, Acor_av=0.784 F test: Probability=0.000, F= 0.623 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04518, wR= 0.06042, Acormin=0.505, Acormax=1.070, Acor_av=0.706 F test: Probability=0.000, F= 0.905 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03758, wR= 0.05287, Acormin=0.479, Acormax=1.152, Acor_av=0.753 F test: Probability=1.000, F= 1.300 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03475, wR= 0.04874, Acormin=0.466, Acormax=1.210, Acor_av=0.777 F test: Probability=0.998, F= 1.158 Final absorption model (ne=8, no=7): Rint= 0.03475, Acormin=0.466, Acormax=1.210, Acor_av=0.777 Combined refinement in use Rint: 0.11119 There are 74 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13895 Using Levenberg-Marquardt: 0.00010 New wR= 0.04233 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11105 with corrections 0.03010 Rint for all data: 0.11119 with corrections 0.03032 4 observations identified as outliers and rejected Cycle 2 wR= 0.03901 Using Levenberg-Marquardt: 0.00001 New wR= 0.03743 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11064 with corrections 0.02697 Rint for all data: 0.11119 with corrections 0.03004 2 observations identified as outliers and rejected Cycle 3 wR= 0.03603 Using Levenberg-Marquardt: 0.00000 New wR= 0.03570 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11061 with corrections 0.02637 Rint for all data: 0.11119 with corrections 0.02999 0 observations identified as outliers and rejected Cycle 4 wR= 0.03570 Using Levenberg-Marquardt: 0.00000 New wR= 0.03558 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11061 with corrections 0.02638 Rint for all data: 0.11119 with corrections 0.02992 0 observations identified as outliers and rejected Cycle 5 wR= 0.03558 Using Levenberg-Marquardt: 0.00000 New wR= 0.03553 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.11061 with corrections 0.02641 Rint for all data: 0.11119 with corrections 0.02989 0 observations identified as outliers and rejected Final wR= 0.03553 Final frame scales: Min= 0.8515 Max= 1.1636 Final absorption correction factors: Amin= 0.5750 Amax= 1.2905 PROFFIT INFO: Inet (after scale3 abspack): min=821.6105 max=6283280.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=115.7361 max=48856.8086 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2106 reflections read from tmp file 233 reflections are rejected (231 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 5 0 4 7 4 2 1 82 Initial Chi^2= 0.30956 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.27862 Current error model SIG(F2)^2 = 133.07*I_RAW + 0.00*I_BACK+(0.00064*)^2 Negative value encountered! Resetting parameters to initial values... Cycle 2, Chi^2= 1.28425 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02540*)^2 Cycle 3, Chi^2= 1.36141 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02340*)^2 Cycle 4, Chi^2= 1.38462 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02285*)^2 Cycle 5, Chi^2= 1.39126 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02269*)^2 Cycle 6, Chi^2= 1.39312 Current error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02265*)^2 Final Chi^2= 1.39312 Final error model SIG(F2)^2 = 42.86*I_RAW + 0.00*I_BACK+(0.02265*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6283280- 1219601 210 1987908.28 43.18 100.00 1209034- 680583 210 901257.99 40.76 100.00 678902- 297732 210 460188.51 39.75 100.00 297643- 175334 210 217925.61 37.27 100.00 175315- 141308 210 158560.43 33.40 100.00 140977- 98050 210 112664.99 28.36 100.00 97977- 77650 210 88681.09 25.35 100.00 77545- 5716 210 45259.65 19.30 100.00 5697- 3164 210 4162.05 7.69 100.00 3159- 822 216 2448.52 6.53 99.54 ------------------------------------------------------------------------------------ 6283280- 822 2106 396779.05 28.10 99.95 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 210 786979.23 37.26 100.00 1.39- 1.12 210 803568.32 32.87 100.00 1.12- 0.96 210 399183.38 31.36 100.00 0.96- 0.88 210 400602.86 29.02 100.00 0.85- 0.81 210 476870.26 32.20 100.00 0.81- 0.73 210 260809.54 24.22 100.00 0.73- 0.70 210 183829.34 22.74 99.52 0.70- 0.65 210 332533.05 29.09 100.00 0.65- 0.62 210 168074.53 21.22 100.00 0.62- 0.58 216 162046.67 21.21 100.00 ------------------------------------------------------------------------------------ 4.82- 0.58 2106 396779.05 28.10 99.95 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 210 786979.23 37.26 100.00 4.82- 1.12 420 795273.77 35.06 100.00 4.82- 0.96 630 663243.64 33.83 100.00 4.82- 0.88 840 597583.44 32.63 100.00 4.82- 0.81 1050 573440.81 32.54 100.00 4.82- 0.73 1260 521335.60 31.15 100.00 4.82- 0.70 1470 473120.42 29.95 99.93 4.82- 0.65 1680 455547.00 29.84 99.94 4.82- 0.62 1890 423605.61 28.89 99.95 4.82- 0.58 2106 396779.05 28.10 99.95 ------------------------------------------------------------------------------------ 4.82- 0.58 2106 396779.05 28.10 99.95 Scale applied to data: s=0.159152 (maximum obs:6283280.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.025: data 2106 -> merged 110 With outlier rejection... Rint 0.026; Rsigma 0.025: data 2088 -> merged 110 Rejected total: 18, method kkm 18, method Blessing 0 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585949, 4.831857 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 11.40 100.00 114 1.61 - 1.21 10 10 19.00 100.00 190 1.17 - 1.01 10 10 24.40 100.00 244 0.99 - 0.89 10 10 24.30 100.00 243 0.88 - 0.81 10 10 23.60 100.00 236 0.81 - 0.74 10 10 20.00 100.00 200 0.73 - 0.71 10 10 22.70 100.00 227 0.70 - 0.66 10 10 18.70 100.00 187 0.66 - 0.64 10 10 17.40 100.00 174 0.63 - 0.60 10 10 16.90 100.00 169 --------------------------------------------------------------- 5.92 - 0.60 100 100 19.84 100.00 1984 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:45:46 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917173 5.917888 5.916754 60.0377 90.0596 60.0132 1959 Reflections read from file xs1714a.hkl; mean (I/sigma) = 27.98 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 963 1049 968 983 1490 1311 1319 1959 N (int>3sigma) = 0 845 1049 850 859 1372 1154 1147 1714 Mean intensity = 0.0 57.8 29.4 57.3 64.8 47.6 69.6 67.1 67.1 Mean int/sigma = 0.0 26.3 23.8 25.7 27.2 25.2 29.0 28.4 28.0 Lattice type: P chosen Volume: 146.54 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 Unitcell: 5.915 5.917 5.917 90.06 119.95 119.97 Niggli form: a.a = 34.992 b.b = 35.008 c.c = 35.013 b.c = -0.036 a.c = -17.475 a.b = -17.484 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.060 CUBIC F-lattice R(int) = 0.176 [ 1806] Vol = 586.2 Cell: 8.372 8.371 8.363 90.02 90.00 90.02 Volume: 586.16 Matrix:-1.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.165 [ 1531] Vol = 439.6 Cell: 5.919 5.917 14.500 90.05 90.00 120.03 Volume: 439.62 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.058 RHOMBOHEDRAL R-lattice R(int) = 0.153 [ 481] Vol = 439.6 Trigonal Cell: 5.919 5.917 14.500 90.05 90.00 120.03 Volume: 439.62 Matrix:-1.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.028 TETRAGONAL I-lattice R(int) = 0.152 [ 1567] Vol = 293.1 Cell: 5.921 5.919 8.363 89.99 89.98 90.01 Volume: 293.08 Matrix: 0.0000 1.0000 -1.0000 -1.0000 1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.021 TETRAGONAL I-lattice R(int) = 0.152 [ 1567] Vol = 293.1 Cell: 5.919 5.921 8.363 90.02 90.01 90.01 Volume: 293.08 Matrix:-1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 1519] Vol = 293.1 Cell: 5.919 5.921 8.363 89.98 89.99 90.01 Volume: 293.08 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.024 ORTHORHOMBIC I-lattice R(int) = 0.151 [ 1517] Vol = 293.1 Cell: 5.915 8.372 5.918 89.98 89.95 89.99 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.017 MONOCLINIC I-lattice R(int) = 0.147 [ 1209] Vol = 293.1 Cell: 5.921 5.919 8.363 90.01 90.02 90.01 Volume: 293.08 Matrix: 0.0000 -1.0000 1.0000 1.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.034 MONOCLINIC I-lattice R(int) = 0.137 [ 1205] Vol = 293.1 Cell: 5.915 5.918 8.372 90.02 90.01 89.95 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.012 MONOCLINIC I-lattice R(int) = 0.131 [ 1229] Vol = 293.1 Cell: 5.915 8.372 5.918 89.98 90.05 90.01 Volume: 293.08 Matrix: 1.0000 -1.0000 1.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.024 MONOCLINIC I-lattice R(int) = 0.135 [ 1208] Vol = 293.1 Cell: 5.918 5.915 8.372 89.99 90.02 90.05 Volume: 293.08 Matrix: 0.0000 -1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.050 MONOCLINIC C-lattice R(int) = 0.140 [ 1250] Vol = 293.1 Cell: 10.249 5.917 5.917 90.06 125.23 89.96 Volume: 293.08 Matrix:-2.0000 2.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.115 [ 756] Vol = 146.5 Cell: 5.915 5.917 5.917 90.06 119.95 119.97 Volume: 146.54 Matrix:-1.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 1.0000 0.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1049 0 1312 1311 1959 N (int>3sigma) = 0 0 0 0 1049 0 1151 1154 1714 Mean intensity = 0.0 0.0 0.0 0.0 29.4 0.0 67.3 69.6 67.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 27.9 29.0 28.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.130 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 20 20 143 448 N I>3s 19 19 90 448 0.8 0.8 0.7 34.3 6.3 6.3 3.9 29.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.176 1682 Fd-3m 1 1 227 C N N N N 37 2284 0.178 1720 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.372201 8.371245 8.363497 90.0245 89.9959 90.0192 ZERR 1.00 0.001766 0.003921 0.000304 0.0129 0.0018 0.0024 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4827908- 608008 471 466 27 17.3 1340783.23 41.54 0.023 0.027 570189- 136080 617 615 27 22.8 240527.37 36.30 0.030 0.036 117556- 40776 525 524 27 19.4 87699.73 25.26 0.043 0.055 11411- 1975 493 483 29 16.7 3870.39 7.70 0.135 0.162 ------------------------------------------------------------------------------------------- 4827908- 1975 2106 2088 110 19.0 392985.33 28.09 0.026 0.030 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 516 506 27 18.7 697495.63 35.20 0.023 0.027 0.024 1.01-0.78 646 641 28 22.9 375680.61 27.56 0.022 0.026 0.025 0.76-0.65 564 562 28 20.1 279006.35 25.71 0.030 0.035 0.027 0.65-0.59 380 379 27 14.0 184716.99 23.00 0.044 0.046 0.031 ------------------------------------------------------------------------------------------------------ inf-0.59 2106 2088 110 19.0 392985.33 28.09 0.026 0.030 0.025 inf-0.60 1999 1982 99 20.0 406982.38 28.48 0.025 0.030 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 506 27 27 100.0 18.7 697495.63 176.53 0.023 0.009 1.01-0.78 641 28 28 100.0 22.9 375680.61 145.33 0.022 0.006 0.76-0.65 562 28 28 100.0 20.1 279006.35 124.73 0.030 0.007 0.65-0.59 379 27 27 100.0 14.0 184716.99 100.67 0.044 0.011 -------------------------------------------------------------------------------------------- inf-0.59 2088 110 110 100.0 19.0 392985.33 139.24 0.026 0.008 inf-0.60 1982 99 99 100.0 20.0 406982.38 142.17 0.025 0.008 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 14:52:42 2018) ID: 2932; threads 39; handles 878; mem 518720.00 (1237700.00)kB; time: 1w 4d 23h 58m 12s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 697.1, WS: 297.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.4,peak PF: 697.1, WS: 299.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 14:52:42 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000013 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000015 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) 5.91502 ( 0.00083 ) 5.91640 ( 0.00083 ) 5.92265 ( 0.00064 ) 60.05206 ( 0.01291 ) 89.98756 ( 0.00996 ) 60.01743 ( 0.01461 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 14:52:42 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000013 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000015 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021559 -0.014369 0.007200 ( 0.000004 0.000003 0.000002 ) -0.014369 0.028717 -0.014360 ( 0.000003 0.000004 0.000002 ) 0.007200 -0.014360 0.021552 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(13) 89.988(10) 60.017(15) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb PROFFITPEAK info: 998 peaks in the peak location table UB fit with 441 obs out of 466 (total:466,skipped:0) (94.64%) UB - matrix: -0.069828 0.031211 0.088967 ( 0.000054 0.000105 0.000069 ) -0.068681 -0.065663 -0.010066 ( 0.000054 0.000106 0.000069 ) 0.108997 -0.153038 0.116433 ( 0.000062 0.000121 0.000079 ) M - matrix: 0.021473 -0.014350 0.007170 ( 0.000017 0.000020 0.000014 ) -0.014350 0.028706 -0.014381 ( 0.000020 0.000040 0.000021 ) 0.007170 -0.014381 0.021573 ( 0.000014 0.000021 0.000022 ) unit cell: 5.932(5) 5.927(5) 5.917(4) 59.95(8) 89.92(6) 59.94(9) V = 146.94(17) UB fit with 441 obs out of 466 (total:466,skipped:0) (94.64%) UB - matrix: -0.069828 0.031211 0.088967 ( 0.000054 0.000105 0.000069 ) -0.068681 -0.065663 -0.010066 ( 0.000054 0.000106 0.000069 ) 0.108997 -0.153038 0.116433 ( 0.000062 0.000121 0.000079 ) M - matrix: 0.021473 -0.014350 0.007170 ( 0.000017 0.000020 0.000014 ) -0.014350 0.028706 -0.014381 ( 0.000020 0.000040 0.000021 ) 0.007170 -0.014381 0.021573 ( 0.000014 0.000021 0.000022 ) unit cell: 5.932(5) 5.927(5) 5.917(4) 59.95(8) 89.92(6) 59.94(9) V = 146.94(17) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.069917 0.031213 0.088895 ( 0.000051 0.000101 0.000066 ) -0.068706 -0.065581 -0.010054 ( 0.000051 0.000101 0.000065 ) 0.108757 -0.152958 0.116362 ( 0.000067 0.000132 0.000085 ) M - matrix: 0.021437 -0.014312 0.007131 ( 0.000018 0.000021 0.000014 ) -0.014312 0.028671 -0.014364 ( 0.000021 0.000043 0.000023 ) 0.007131 -0.014364 0.021543 ( 0.000014 0.000023 0.000023 ) UB fit with 436 obs out of 466 (total:466,skipped:0) (93.56%) unit cell: 5.933(5) 5.930(5) 5.922(4) 59.89(8) 89.84(6) 59.95(8) V = 147.17(17) UB fit with 436 obs out of 466 (total:466,skipped:0) (93.56%) UB - matrix: -0.069917 0.031213 0.088895 ( 0.000051 0.000101 0.000066 ) -0.068706 -0.065581 -0.010054 ( 0.000051 0.000101 0.000065 ) 0.108757 -0.152958 0.116362 ( 0.000067 0.000132 0.000085 ) M - matrix: 0.021437 -0.014312 0.007131 ( 0.000018 0.000021 0.000014 ) -0.014312 0.028671 -0.014364 ( 0.000021 0.000043 0.000023 ) 0.007131 -0.014364 0.021543 ( 0.000014 0.000023 0.000023 ) unit cell: 5.933(5) 5.930(5) 5.922(4) 59.89(8) 89.84(6) 59.95(8) V = 147.17(17) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.069950 0.031202 0.088893 ( 0.000051 0.000101 0.000065 ) -0.068719 -0.065551 -0.010083 ( 0.000051 0.000101 0.000065 ) 0.108717 -0.152933 0.116327 ( 0.000067 0.000132 0.000085 ) M - matrix: 0.021435 -0.014304 0.007121 ( 0.000018 0.000021 0.000014 ) -0.014304 0.028659 -0.014356 ( 0.000021 0.000043 0.000023 ) 0.007121 -0.014356 0.021535 ( 0.000014 0.000023 0.000023 ) UB fit with 436 obs out of 466 (total:466,skipped:0) (93.56%) unit cell: 5.933(5) 5.931(5) 5.922(4) 59.89(8) 89.82(6) 59.95(8) V = 147.21(17) 466 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Run 4 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 586 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069950 0.031202 0.088893 ( 0.000051 0.000101 0.000065 ) -0.068719 -0.065551 -0.010083 ( 0.000051 0.000101 0.000065 ) 0.108717 -0.152933 0.116327 ( 0.000067 0.000132 0.000085 ) M - matrix: 0.021435 -0.014304 0.007121 ( 0.000018 0.000021 0.000014 ) -0.014304 0.028659 -0.014356 ( 0.000021 0.000043 0.000023 ) 0.007121 -0.014356 0.021535 ( 0.000014 0.000023 0.000023 ) UB fit with 436 obs out of 466 (total:466,skipped:0) (93.56%) unit cell: 5.933(5) 5.931(5) 5.922(4) 59.89(8) 89.82(6) 59.95(8) V = 147.21(17) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 432 obs out of 466 (total:466,skipped:0) (92.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb 8 of 338 peaks identified as outliers and rejected 330 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 330 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 330 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 1.41 | 33 | 1.007 ( 0.096) | 1.068 ( 0.244) | 1.125 ( 0.549) | 1.41- 1.15 | 33 | 1.056 ( 0.094) | 1.282 ( 0.600) | 1.183 ( 0.701) | 1.12- 0.98 | 33 | 1.015 ( 0.103) | 1.048 ( 0.163) | 1.001 ( 0.340) | 0.98- 0.89 | 33 | 1.020 ( 0.097) | 1.016 ( 0.143) | 1.127 ( 0.430) | 0.89- 0.82 | 33 | 1.042 ( 0.075) | 1.005 ( 0.109) | 1.288 ( 0.558) | 0.82- 0.75 | 33 | 1.023 ( 0.086) | 0.989 ( 0.136) | 1.080 ( 0.416) | 0.75- 0.71 | 33 | 1.020 ( 0.044) | 0.948 ( 0.113) | 1.309 ( 0.548) | 0.71- 0.66 | 33 | 0.991 ( 0.042) | 0.889 ( 0.082) | 1.182 ( 0.457) | 0.66- 0.62 | 33 | 0.966 ( 0.039) | 0.846 ( 0.041) | 1.212 ( 0.468) | 0.62- 0.59 | 33 | 0.939 ( 0.044) | 0.800 ( 0.034) | 1.266 ( 0.477) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 0.59 | 330 | 1.008 ( 0.083) | 0.989 ( 0.261) | 1.177 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) UB - matrix: -0.070178 0.031430 0.088659 ( 0.000018 0.000037 0.000026 ) -0.068839 -0.065708 -0.010263 ( 0.000022 0.000043 0.000031 ) 0.108855 -0.152843 0.116149 ( 0.000015 0.000031 0.000022 ) M - matrix: 0.021513 -0.014320 0.007128 ( 0.000005 0.000006 0.000004 ) -0.014320 0.028666 -0.014292 ( 0.000006 0.000011 0.000006 ) 0.007128 -0.014292 0.021456 ( 0.000004 0.000006 0.000007 ) unit cell: 5.9192(19) 5.9189(19) 5.9250(14) 60.04(3) 89.95(2) 60.00(3) V = 146.92(6) OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 OTKP changes: 330 1 1 1 UB - matrix: -0.069901 0.031369 0.088707 ( 0.000017 0.000034 0.000024 ) -0.068742 -0.065773 -0.010009 ( 0.000019 0.000038 0.000027 ) 0.108912 -0.152889 0.116265 ( 0.000015 0.000030 0.000021 ) M - matrix: 0.021473 -0.014323 0.007150 ( 0.000005 0.000005 0.000004 ) -0.014323 0.028685 -0.014335 ( 0.000005 0.000011 0.000006 ) 0.007150 -0.014335 0.021487 ( 0.000004 0.000006 0.000007 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9269(17) 5.9226(17) 5.9266(13) 59.98(3) 89.97(2) 60.00(3) V = 147.11(6) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 586 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069901 0.031369 0.088707 ( 0.000017 0.000034 0.000024 ) -0.068742 -0.065773 -0.010009 ( 0.000019 0.000038 0.000027 ) 0.108912 -0.152889 0.116265 ( 0.000015 0.000030 0.000021 ) M - matrix: 0.021473 -0.014323 0.007150 ( 0.000005 0.000005 0.000004 ) -0.014323 0.028685 -0.014335 ( 0.000005 0.000011 0.000006 ) 0.007150 -0.014335 0.021487 ( 0.000004 0.000006 0.000007 ) UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) unit cell: 5.9269(17) 5.9226(17) 5.9266(13) 59.98(3) 89.97(2) 60.00(3) V = 147.11(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 330 obs out of 330 (total:330,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb 5 of 336 peaks identified as outliers and rejected 331 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 331 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 331 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 1.41 | 33 | 1.024 ( 0.171) | 1.144 ( 0.498) | 1.218 ( 0.874) | 1.41- 1.15 | 33 | 1.051 ( 0.089) | 1.212 ( 0.501) | 1.187 ( 0.702) | 1.12- 0.99 | 33 | 1.013 ( 0.109) | 1.029 ( 0.129) | 0.986 ( 0.354) | 0.98- 0.89 | 33 | 1.029 ( 0.091) | 1.024 ( 0.140) | 1.166 ( 0.454) | 0.88- 0.82 | 33 | 1.035 ( 0.079) | 1.010 ( 0.119) | 1.243 ( 0.542) | 0.81- 0.75 | 33 | 1.029 ( 0.082) | 0.991 ( 0.132) | 1.123 ( 0.461) | 0.75- 0.71 | 33 | 1.016 ( 0.046) | 0.948 ( 0.118) | 1.299 ( 0.538) | 0.70- 0.66 | 33 | 0.995 ( 0.041) | 0.893 ( 0.085) | 1.178 ( 0.455) | 0.66- 0.63 | 33 | 0.965 ( 0.041) | 0.845 ( 0.043) | 1.213 ( 0.477) | 0.63- 0.59 | 34 | 0.944 ( 0.043) | 0.803 ( 0.036) | 1.267 ( 0.464) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 0.59 | 331 | 1.010 ( 0.094) | 0.989 ( 0.271) | 1.188 ( 0.557) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 166 | 1.119 ( 0.119) | 1.243 ( 0.466) | 1.187 ( 0.623) | 13.3-19.0 | 166 | 1.081 ( 0.052) | 1.130 ( 0.250) | 1.232 ( 0.537) | 19.0-23.3 | 166 | 1.071 ( 0.075) | 1.154 ( 0.401) | 1.184 ( 0.516) | 23.3-27.2 | 166 | 1.034 ( 0.080) | 1.075 ( 0.292) | 1.205 ( 0.582) | 27.2-30.9 | 166 | 1.013 ( 0.077) | 1.004 ( 0.174) | 1.214 ( 0.511) | 30.9-33.8 | 166 | 0.984 ( 0.086) | 0.924 ( 0.098) | 1.181 ( 0.512) | 33.9-36.9 | 166 | 0.968 ( 0.077) | 0.902 ( 0.097) | 1.189 ( 0.490) | 36.9-39.7 | 166 | 0.946 ( 0.093) | 0.877 ( 0.146) | 1.156 ( 0.537) | 39.8-42.8 | 166 | 0.927 ( 0.084) | 0.836 ( 0.082) | 1.176 ( 0.510) | 42.8-49.9 | 164 | 0.938 ( 0.082) | 0.816 ( 0.065) | 1.161 ( 0.454) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1658 | 1.008 ( 0.105) | 0.996 ( 0.284) | 1.188 ( 0.530) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0010 b=1.04 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3686101 PROFFITPEAK - Finished at Tue Mar 27 14:53:00 2018 PROFFITMAIN - Started at Tue Mar 27 14:53:00 2018 OTKP changes: 1658 2 3 4 OTKP changes: 1658 2 3 4 UB - matrix: -0.070177 0.031088 0.088928 ( 0.000012 0.000012 0.000012 ) -0.068713 -0.065901 -0.010450 ( 0.000012 0.000013 0.000012 ) 0.109155 -0.153022 0.116316 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021561 -0.014357 0.007174 ( 0.000003 0.000002 0.000002 ) -0.014357 0.028725 -0.014346 ( 0.000002 0.000004 0.000002 ) 0.007174 -0.014346 0.021547 ( 0.000002 0.000002 0.000003 ) UB fit with 1658 obs out of 1658 (total:1658,skipped:0) (100.00%) unit cell: 5.9137(7) 5.9135(7) 5.9144(6) 60.043(12) 90.016(9) 60.022(13) V = 146.38(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070039 0.030657 0.088975 ( 0.000029 0.000028 0.000016 ) -0.068253 -0.066143 -0.010487 ( 0.000026 0.000025 0.000015 ) 0.109063 -0.153048 0.115956 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021459 -0.014325 0.007130 ( 0.000008 0.000006 0.000004 ) -0.014325 0.028738 -0.014325 ( 0.000006 0.000008 0.000005 ) 0.007130 -0.014325 0.021472 ( 0.000004 0.000005 0.000004 ) unit cell: 5.9276(14) 5.9136(14) 5.9250(11) 60.01(2) 89.960(18) 60.00(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070317 0.030926 0.088796 ( 0.000026 0.000026 0.000015 ) -0.068407 -0.066117 -0.010695 ( 0.000024 0.000023 0.000013 ) 0.109321 -0.153274 0.116355 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021575 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028821 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9165(13) 5.9080(13) 5.9187(10) 60.05(2) 90.074(16) 60.00(2) V = 146.31(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.802) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070317 0.030926 0.088796 ( 0.000026 0.000026 0.000015 ) -0.068407 -0.066117 -0.010695 ( 0.000024 0.000023 0.000013 ) 0.109321 -0.153274 0.116355 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021575 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028821 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9165(13) 5.9080(13) 5.9187(10) 60.05(2) 90.074(16) 60.00(2) V = 146.31(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070317 0.030926 0.088796 ( 0.000026 0.000026 0.000015 ) -0.068407 -0.066117 -0.010695 ( 0.000024 0.000023 0.000013 ) 0.109321 -0.153274 0.116355 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021575 -0.014408 0.007208 ( 0.000007 0.000005 0.000004 ) -0.014408 0.028821 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007208 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9165(13) 5.9080(13) 5.9187(10) 60.05(2) 90.074(16) 60.00(2) V = 146.31(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031361 0.088643 ( 0.000026 0.000023 0.000028 ) -0.068572 -0.066013 -0.010220 ( 0.000031 0.000027 0.000033 ) 0.108984 -0.152621 0.116241 ( 0.000020 0.000017 0.000022 ) M - matrix: 0.021537 -0.014315 0.007128 ( 0.000007 0.000005 0.000005 ) -0.014315 0.028634 -0.014286 ( 0.000005 0.000007 0.000005 ) 0.007128 -0.014286 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(17) 5.9211(17) 5.9219(14) 60.03(3) 89.94(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070353 0.031193 0.088837 ( 0.000023 0.000020 0.000025 ) -0.068771 -0.065860 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109158 -0.153138 0.116565 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021594 -0.014381 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014381 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014398 0.021586 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9101(16) 5.9170(16) 5.9152(12) 59.94(2) 89.945(19) 60.01(3) V = 146.21(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.802) HKL list info: 721 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070353 0.031193 0.088837 ( 0.000023 0.000020 0.000025 ) -0.068771 -0.065860 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109158 -0.153138 0.116565 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021594 -0.014381 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014381 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014398 0.021586 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9101(16) 5.9170(16) 5.9152(12) 59.94(2) 89.945(19) 60.01(3) V = 146.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070353 0.031193 0.088837 ( 0.000023 0.000020 0.000025 ) -0.068771 -0.065860 -0.010344 ( 0.000030 0.000026 0.000032 ) 0.109158 -0.153138 0.116565 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021594 -0.014381 0.007185 ( 0.000007 0.000005 0.000005 ) -0.014381 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007185 -0.014398 0.021586 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9101(16) 5.9170(16) 5.9152(12) 59.94(2) 89.945(19) 60.01(3) V = 146.21(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 331 obs out of 331 (total:331,skipped:0) (100.00%) UB - matrix: -0.070175 0.031451 0.088650 ( 0.000018 0.000036 0.000026 ) -0.068836 -0.065730 -0.010269 ( 0.000023 0.000046 0.000033 ) 0.108889 -0.152846 0.116164 ( 0.000015 0.000031 0.000022 ) M - matrix: 0.021520 -0.014326 0.007135 ( 0.000005 0.000006 0.000004 ) -0.014326 0.028672 -0.014292 ( 0.000006 0.000011 0.000006 ) 0.007135 -0.014292 0.021458 ( 0.000004 0.000006 0.000007 ) unit cell: 5.919(2) 5.918(2) 5.9244(14) 60.05(3) 89.98(2) 60.00(3) V = 146.88(7) OTKP changes: 331 1 1 1 OTKP changes: 331 1 1 1 OTKP changes: 331 1 1 1 UB - matrix: -0.070101 0.031402 0.088900 ( 0.000017 0.000034 0.000024 ) -0.068693 -0.066079 -0.009996 ( 0.000020 0.000041 0.000029 ) 0.109192 -0.153120 0.116565 ( 0.000015 0.000030 0.000021 ) M - matrix: 0.021556 -0.014382 0.007183 ( 0.000005 0.000006 0.000004 ) -0.014382 0.028798 -0.014396 ( 0.000006 0.000011 0.000006 ) 0.007183 -0.014396 0.021590 ( 0.000004 0.000006 0.000007 ) UB fit with 331 obs out of 331 (total:331,skipped:0) (100.00%) unit cell: 5.9163(18) 5.9112(18) 5.9121(13) 59.99(3) 89.97(2) 60.00(3) V = 146.20(6) Run 4 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.802) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070101 0.031402 0.088900 ( 0.000017 0.000034 0.000024 ) -0.068693 -0.066079 -0.009996 ( 0.000020 0.000041 0.000029 ) 0.109192 -0.153120 0.116565 ( 0.000015 0.000030 0.000021 ) M - matrix: 0.021556 -0.014382 0.007183 ( 0.000005 0.000006 0.000004 ) -0.014382 0.028798 -0.014396 ( 0.000006 0.000011 0.000006 ) 0.007183 -0.014396 0.021590 ( 0.000004 0.000006 0.000007 ) UB fit with 331 obs out of 331 (total:331,skipped:0) (100.00%) unit cell: 5.9163(18) 5.9112(18) 5.9121(13) 59.99(3) 89.97(2) 60.00(3) V = 146.20(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 331 obs out of 331 (total:331,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070101 0.031402 0.088900 ( 0.000017 0.000034 0.000024 ) -0.068693 -0.066079 -0.009996 ( 0.000020 0.000041 0.000029 ) 0.109192 -0.153120 0.116565 ( 0.000015 0.000030 0.000021 ) M - matrix: 0.021556 -0.014382 0.007183 ( 0.000005 0.000006 0.000004 ) -0.014382 0.028798 -0.014396 ( 0.000006 0.000011 0.000006 ) 0.007183 -0.014396 0.021590 ( 0.000004 0.000006 0.000007 ) UB fit with 331 obs out of 331 (total:331,skipped:0) (100.00%) unit cell: 5.9163(18) 5.9112(18) 5.9121(13) 59.99(3) 89.97(2) 60.00(3) V = 146.20(6) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070072 0.031056 0.088879 ( 0.000012 0.000013 0.000012 ) -0.068691 -0.065794 -0.010502 ( 0.000014 0.000015 0.000014 ) 0.109196 -0.153060 0.116392 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021552 -0.014370 0.007203 ( 0.000003 0.000003 0.000002 ) -0.014370 0.028721 -0.014364 ( 0.000003 0.000004 0.000002 ) 0.007203 -0.014364 0.021557 ( 0.000002 0.000002 0.000003 ) UB fit with 1658 obs out of 1658 (total:1658,skipped:0) (100.00%) unit cell: 5.9186(8) 5.9179(8) 5.9163(6) 60.039(13) 90.065(10) 60.011(14) V = 146.56(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 58 reflections under beam stop or inside a detector rejection region 14 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof 2256 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 14:53:04 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.802) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.802) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.802) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2952906.1424 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4724650.0000 PROFFIT INFO: sig(Inet): min=96.4225 max=47444.6406 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=228.95 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 12 81 208 454 507 883 1483 2057 2256 Percent 0.0 0.0 0.5 3.6 9.2 20.1 22.5 39.1 65.7 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2256 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2256 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4724650- 1221832 225 1960481.35 121.67 100.00 1217769- 711707 225 929753.53 106.80 100.00 706834- 281108 225 462251.48 97.53 100.00 280291- 180834 225 216856.76 74.26 100.00 180524- 136011 225 158578.20 52.41 100.00 135852- 102257 225 116460.04 37.48 100.00 102256- 78746 225 90654.24 30.31 100.00 78653- 5997 225 45789.25 20.86 100.00 5937- 3260 225 4307.93 5.59 97.78 3246- 924 231 2438.63 4.16 67.10 ------------------------------------------------------------------------------------ 4724650- 924 2256 397703.10 54.97 96.41 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 225 701186.52 87.64 99.11 1.41- 1.07 225 622564.26 69.43 97.78 1.07- 0.96 225 415346.37 60.56 98.22 0.93- 0.82 225 451765.34 56.71 95.56 0.82- 0.74 225 399133.39 56.69 97.33 0.74- 0.69 225 333458.95 50.86 96.44 0.69- 0.63 225 310837.66 49.37 97.33 0.63- 0.57 225 306086.15 46.16 92.44 0.57- 0.52 225 245953.97 39.69 95.56 0.52- 0.40 231 196075.15 33.19 94.37 ------------------------------------------------------------------------------------ 5.26- 0.40 2256 397703.10 54.97 96.41 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:53:04 2018 Sorting 2256 observations 260 unique observations with > 7.00 F2/sig(F2) 2256 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 74 388 Total number of frames 388 Maximum number of 260 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2256 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 37 197 Total number of frames 197 1822 observations > 7.00 F2/sig(F2) 1822 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 37 197 Total number of frames 197 Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 1822 removed 53 = 1769, unique = 245) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1769 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 37 197 Total number of frames 197 245 unique data precomputed (should be 245) 245 unique data with 1769 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 1769 removed 0 = 1769, unique = 245) 245 unique data precomputed (should be 245) 245 unique data with 1769 observations RMS deviation of equivalent data = 0.71585 Rint = 0.69261 11 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.67033, wR= 3.63172 Trying model 1 (ne=2, no=0)... Results: Rint= 0.73689, wR= 2.67871, Acormin=-0.066, Acormax=2.019, Acor_av=0.642 F test: Probability=0.000, F= 0.825 Trying model 2 (ne=2, no=1)... Results: Rint= 0.90236, wR= 2.58877, Acormin=-0.501, Acormax=1.879, Acor_av=0.356 F test: Probability=0.000, F= 0.549 Trying model 3 (ne=4, no=0)... Results: Rint= 0.75022, wR= 2.18397, Acormin=-0.090, Acormax=2.363, Acor_av=0.526 F test: Probability=0.000, F= 0.791 Trying model 4 (ne=4, no=1)... Results: Rint= 0.90809, wR= 2.17137, Acormin=-0.439, Acormax=2.054, Acor_av=0.292 F test: Probability=0.000, F= 0.539 Trying model 5 (ne=4, no=3)... Results: Rint= 0.97509, wR= 1.91317, Acormin=-1.176, Acormax=1.616, Acor_av=0.142 F test: Probability=0.000, F= 0.465 Trying model 6 (ne=6, no=0)... Results: Rint= 0.79156, wR= 2.27029, Acormin=-0.213, Acormax=2.896, Acor_av=0.435 F test: Probability=0.000, F= 0.704 Trying model 7 (ne=6, no=1)... Results: Rint= 0.93576, wR= 2.26758, Acormin=-0.655, Acormax=2.344, Acor_av=0.218 F test: Probability=0.000, F= 0.503 Trying model 8 (ne=6, no=3)... Results: Rint= 0.98034, wR= 2.17987, Acormin=-1.330, Acormax=1.652, Acor_av=0.107 F test: Probability=0.000, F= 0.456 Trying model 9 (ne=6, no=5)... Results: Rint= 0.98804, wR= 2.20228, Acormin=-1.138, Acormax=2.093, Acor_av=0.080 F test: Probability=0.000, F= 0.446 Trying model 10 (ne=8, no=0)... Results: Rint= 0.87353, wR= 2.10581, Acormin=-0.662, Acormax=3.096, Acor_av=0.328 F test: Probability=0.000, F= 0.572 Trying model 11 (ne=8, no=1)... Results: Rint= 1.00947, wR= 1.78074, Acormin=-1.277, Acormax=1.586, Acor_av=0.064 F test: Probability=0.000, F= 0.427 Trying model 12 (ne=8, no=3)... Results: Rint= 0.99656, wR= 1.55631, Acormin=-0.040, Acormax=0.081, Acor_av=0.001 F test: Probability=0.000, F= 0.436 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99921, wR= 1.59641, Acormin=-0.042, Acormax=0.091, Acor_av=0.002 F test: Probability=0.000, F= 0.431 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00476, wR= 1.55485, Acormin=-0.040, Acormax=0.089, Acor_av=0.001 F test: Probability=0.000, F= 0.422 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86048 There are 197 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 201 pars with 20301 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71585 Using Levenberg-Marquardt: 0.00010 New wR= 0.69486 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.69261 with corrections 0.66014 Rint for all data: 0.86048 with corrections 0.83738 10 observations identified as outliers and rejected Cycle 2 wR= 0.67285 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.66977 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67265 with corrections 0.64651 Rint for all data: 0.86048 with corrections 0.84326 10 observations identified as outliers and rejected Cycle 3 wR= 0.64437 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64292 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66084 with corrections 0.63587 Rint for all data: 0.86048 with corrections 0.84510 9 observations identified as outliers and rejected Cycle 4 wR= 0.62993 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62826 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65457 with corrections 0.63511 Rint for all data: 0.86048 with corrections 0.84768 8 observations identified as outliers and rejected Cycle 5 wR= 0.61016 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.60825 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65073 with corrections 0.63061 Rint for all data: 0.86048 with corrections 0.84657 7 observations identified as outliers and rejected Final wR= 0.60825 Final frame scales: Min= 0.5224 Max= 1.9433 Final absorption correction factors: Amin= 0.3795 Amax= 1.3208 4 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=776.5131 max=5673958.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=117.9980 max=68826.2109 PROFFIT INFO: 9 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/108 2247 reflections read from tmp file 1737 reflections are rejected (1646 as outliers, 91 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 89 47 18 9 7 2 1 0 1 Initial Chi^2= 0.62634 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.78247 Current error model SIG(F2)^2 = 303.31*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 237.33*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 237.33*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5673958- 1218955 224 1956126.31 96.01 100.00 1218316- 681933 224 904936.43 47.98 100.00 680032- 267615 224 443607.22 44.53 100.00 266732- 175426 224 213043.45 32.85 100.00 174681- 134856 224 153099.87 21.86 100.00 134792- 101312 224 118252.43 18.07 100.00 101291- 72963 224 86868.87 13.77 100.00 72933- 6261 224 43485.60 9.90 96.43 6226- 3182 224 4228.60 3.42 53.13 3177- 777 231 2301.48 2.89 30.74 ------------------------------------------------------------------------------------ 5673958- 777 2247 391379.16 29.05 87.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 224 760532.77 63.12 97.77 1.41- 1.07 224 609812.31 44.05 94.20 1.07- 0.96 224 447618.69 31.65 93.30 0.96- 0.82 224 440406.28 29.34 83.04 0.82- 0.74 224 384436.74 26.74 87.05 0.74- 0.69 224 325731.18 22.59 86.61 0.69- 0.63 224 280853.40 21.43 85.71 0.63- 0.57 224 297257.64 19.98 83.04 0.57- 0.52 224 217177.58 17.44 85.27 0.52- 0.40 231 157280.58 14.58 82.68 ------------------------------------------------------------------------------------ 5.26- 0.40 2247 391379.16 29.05 87.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 224 760532.77 63.12 97.77 5.26- 1.07 448 685172.54 53.59 95.98 5.26- 0.96 672 605987.92 46.28 95.09 5.26- 0.82 896 564592.51 42.04 92.08 5.26- 0.74 1120 528561.36 38.98 91.07 5.26- 0.69 1344 494756.33 36.25 90.33 5.26- 0.63 1568 464198.77 34.13 89.67 5.26- 0.57 1792 443331.13 32.36 88.84 5.26- 0.52 2016 418202.95 30.71 88.44 5.26- 0.40 2247 391379.16 29.05 87.85 ------------------------------------------------------------------------------------ 5.26- 0.40 2247 391379.16 29.05 87.85 Scale applied to data: s=0.176244 (maximum obs:5673958.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.845; Rsigma 0.023: data 2247 -> merged 312 With outlier rejection... Rint 0.755; Rsigma 0.023: data 2078 -> merged 312 Rejected total: 169, method kkm 155, method Blessing 14 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404368, 5.272315 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 10.40 100.00 156 1.46 - 1.12 15 15 16.87 100.00 253 1.08 - 0.96 15 15 14.13 100.00 212 0.96 - 0.86 15 15 13.13 100.00 197 0.86 - 0.79 15 15 11.33 100.00 170 0.79 - 0.73 15 15 10.00 100.00 150 0.73 - 0.69 15 15 8.47 100.00 127 0.69 - 0.65 15 15 8.53 100.00 128 0.65 - 0.63 15 15 5.80 100.00 87 0.63 - 0.60 21 21 5.67 100.00 119 --------------------------------------------------------------- 5.92 - 0.60 156 156 10.25 100.00 1599 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:53:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918594 5.917917 5.916339 60.0386 90.0649 60.0109 2078 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1024 1119 1021 1042 1582 1388 1395 2078 N (int>3sigma) = 0 902 1119 899 915 1460 1230 1220 1824 Mean intensity = 0.0 57.2 28.0 57.1 62.5 46.8 67.8 65.9 65.5 Mean int/sigma = 0.0 27.2 24.1 26.6 27.5 25.9 29.5 29.0 28.6 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.918 119.96 90.05 119.96 Niggli form: a.a = 34.989 b.b = 35.003 c.c = 35.022 b.c = -17.486 a.c = -0.029 a.b = -17.478 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.050 CUBIC F-lattice R(int) = 0.175 [ 1925] Vol = 586.2 Cell: 8.364 8.373 8.371 90.01 89.97 90.02 Volume: 586.22 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.047 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 1652] Vol = 439.7 Cell: 5.916 5.915 14.501 89.97 90.05 119.96 Volume: 439.67 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.047 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 522] Vol = 439.7 Trigonal Cell: 5.916 5.915 14.501 89.97 90.05 119.96 Volume: 439.67 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.053 TETRAGONAL I-lattice R(int) = 0.151 [ 1683] Vol = 293.1 Cell: 5.919 5.921 8.364 89.97 90.00 90.02 Volume: 293.11 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.043 TETRAGONAL I-lattice R(int) = 0.151 [ 1683] Vol = 293.1 Cell: 5.919 5.921 8.364 89.97 90.00 90.02 Volume: 293.11 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.038 ORTHORHOMBIC I-lattice R(int) = 0.150 [ 1632] Vol = 293.1 Cell: 5.919 8.364 5.921 89.97 89.98 90.00 Volume: 293.11 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.014 MONOCLINIC I-lattice R(int) = 0.144 [ 1313] Vol = 293.1 Cell: 8.364 5.919 5.921 90.02 90.03 90.00 Volume: 293.11 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.034 MONOCLINIC I-lattice R(int) = 0.136 [ 1319] Vol = 293.1 Cell: 5.918 5.915 8.373 89.99 90.02 89.95 Volume: 293.11 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.028 MONOCLINIC C-lattice R(int) = 0.130 [ 1335] Vol = 293.1 Cell: 8.364 8.373 5.915 89.99 134.96 90.02 Volume: 293.11 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.112 [ 823] Vol = 146.6 Cell: 5.915 5.916 5.918 119.96 90.05 119.96 Volume: 146.56 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1119 0 1388 1388 2078 N (int>3sigma) = 0 0 0 0 1119 0 1216 1230 1824 Mean intensity = 0.0 0.0 0.0 0.0 28.0 0.0 67.5 67.8 65.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 29.3 29.5 28.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 148 487 N I>3s 20 20 94 487 0.7 0.7 0.7 32.9 5.7 5.7 3.8 30.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 1796 Fd-3m 1 1 227 C N N N N 37 2284 0.177 1834 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363821 8.373300 8.370721 90.0131 89.9736 90.0218 ZERR 1.00 0.000297 0.001715 0.003807 0.0023 0.0125 0.0017 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3217444- 626976 368 344 31 11.1 978936.24 56.58 0.645 0.633 626694- 500499 262 248 31 8.0 557616.04 39.09 0.889 0.744 497885- 381388 240 227 31 7.3 408571.08 33.95 0.854 0.784 378256- 295216 326 315 31 10.2 306403.10 24.50 0.987 1.163 284157- 219667 209 176 31 5.7 184987.51 19.94 0.821 0.814 219427- 164342 252 212 31 6.8 144897.54 20.26 0.591 0.617 162699- 97200 235 220 31 7.1 105320.10 15.84 0.538 0.520 96416- 70275 148 139 31 4.5 85945.20 13.48 0.473 0.297 70191- 50074 118 110 31 3.5 61997.64 10.95 0.424 0.301 49750- 1676 89 87 33 2.6 26258.93 5.99 0.753 0.751 ------------------------------------------------------------------------------------------- 3217444- 1676 2247 2078 312 6.7 371416.08 28.62 0.755 0.728 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 456 430 31 13.9 651976.43 52.54 0.746 0.809 0.013 1.05-0.83 429 413 32 12.9 433431.60 30.29 0.890 1.029 0.021 0.82-0.72 347 334 32 10.4 368955.80 25.77 0.708 0.764 0.026 0.72-0.65 280 254 32 7.9 248733.35 20.14 0.783 0.763 0.031 0.64-0.60 213 186 31 6.0 238875.75 18.51 0.771 0.767 0.034 0.59-0.56 169 155 32 4.8 191193.03 16.20 0.586 0.474 0.038 0.56-0.52 131 109 31 3.5 205590.12 17.49 0.482 0.460 0.038 0.52-0.49 111 97 31 3.1 136062.94 13.12 0.557 0.405 0.046 0.49-0.46 75 65 32 2.0 175866.14 15.57 0.305 0.230 0.043 0.45-0.40 36 35 28 1.3 140898.35 14.33 0.377 0.377 0.044 ------------------------------------------------------------------------------------------------------ inf-0.40 2247 2078 312 6.7 371416.08 28.62 0.755 0.728 0.023 inf-0.60 1705 1599 156 10.3 429559.12 32.46 0.782 0.840 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 430 31 31 100.0 13.9 651976.43 217.79 0.746 0.004 1.05-0.83 413 32 32 100.0 12.9 433431.60 131.19 0.890 0.008 0.82-0.72 334 32 32 100.0 10.4 368955.80 98.52 0.708 0.011 0.72-0.65 254 32 32 100.0 7.9 248733.35 71.70 0.783 0.016 0.64-0.60 186 31 31 100.0 6.0 238875.75 57.65 0.771 0.018 0.59-0.56 155 35 32 91.4 4.8 191193.03 43.78 0.586 0.019 0.56-0.52 109 34 31 91.2 3.5 205590.12 42.00 0.482 0.024 0.52-0.49 97 44 31 70.5 3.1 136062.94 28.86 0.557 0.030 0.49-0.46 65 64 32 50.0 2.0 175866.14 24.96 0.305 0.031 0.45-0.40 35 126 28 22.2 1.3 140898.35 16.99 0.377 0.037 -------------------------------------------------------------------------------------------- inf-0.40 2078 461 312 67.7 6.7 371416.08 108.78 0.755 0.013 inf-0.60 1599 156 156 100.0 10.3 429559.12 130.46 0.782 0.009 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: -0.024931 -0.079474 -0.015528 ( 0.000007 0.000007 0.000006 ) 0.072495 -0.029094 0.032896 ( 0.000008 0.000008 0.000007 ) -0.036264 -0.003598 0.076529 ( 0.000006 0.000006 0.000005 ) M - matrix: 0.007192 0.000003 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007176 0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000002 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024931 -0.079474 -0.015528 ( 0.000007 0.000007 0.000006 ) 0.072495 -0.029094 0.032896 ( 0.000008 0.000008 0.000007 ) -0.036264 -0.003598 0.076529 ( 0.000006 0.000006 0.000005 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3638(7) 8.3734(7) 8.3708(6) 90.013(6) 89.974(6) 90.021(7) V = 586.23(8) unit cell: 8.3693(2) 8.3693(2) 8.3693(2) 90.0 90.0 90.0 V = 586.23(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.802) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.802) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.802) PROFFIT INFO: signal sum: min=237.0000 max=20552300.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2952906.1424 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4724650.0000 PROFFIT INFO: sig(Inet): min=96.4225 max=47444.6406 PROFFIT INFO: Inet/sig(Inet): min=1.03 max=228.95 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 24 162 416 908 1014 1766 2966 4114 4512 Percent 0.0 0.0 0.5 3.6 9.2 20.1 22.5 39.1 65.7 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2256 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2256 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4724650- 1221832 225 1960481.35 121.67 100.00 1217769- 711707 225 929753.53 106.80 100.00 706834- 281108 225 462251.48 97.53 100.00 280291- 180834 225 216856.76 74.26 100.00 180524- 136011 225 158578.20 52.41 100.00 135852- 102257 225 116460.04 37.48 100.00 102256- 78746 225 90654.24 30.31 100.00 78653- 5997 225 45789.25 20.86 100.00 5937- 3260 225 4307.93 5.59 97.78 3246- 924 231 2438.63 4.16 67.10 ------------------------------------------------------------------------------------ 4724650- 924 2256 397703.10 54.97 96.41 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 225 743940.91 94.19 100.00 1.39- 1.12 225 787435.85 65.01 100.00 1.12- 0.96 225 423874.44 69.44 97.78 0.96- 0.88 225 385537.10 62.60 96.44 0.88- 0.81 225 496189.14 71.75 99.56 0.81- 0.73 225 267771.41 42.99 99.56 0.73- 0.71 225 183598.15 33.98 86.67 0.70- 0.65 225 349231.81 50.80 96.89 0.65- 0.62 225 175787.50 30.09 90.22 0.62- 0.58 231 169743.65 29.54 96.97 ------------------------------------------------------------------------------------ 4.82- 0.58 2256 397703.10 54.97 96.41 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 14:53:05 2018 Sorting 2256 observations 85 unique observations with > 7.00 F2/sig(F2) 2256 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 74 388 Total number of frames 388 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2256 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 14 79 Total number of frames 79 1822 observations > 7.00 F2/sig(F2) 1822 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 14 79 Total number of frames 79 Removing 'redundancy=1' reflections Average redundancy: 19.6 (Out of 1822 removed 3 = 1819, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1819 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 14 79 Total number of frames 79 93 unique data precomputed (should be 93) 93 unique data with 1819 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 19.6 (Out of 1819 removed 0 = 1819, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 1819 observations RMS deviation of equivalent data = 0.13789 Rint = 0.10882 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10789, wR= 0.13670 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07864, wR= 0.09674, Acormin=0.805, Acormax=1.243, Acor_av=0.982 F test: Probability=1.000, F= 1.877 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07209, wR= 0.08943, Acormin=0.746, Acormax=1.296, Acor_av=0.954 F test: Probability=1.000, F= 1.188 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06544, wR= 0.08377, Acormin=0.743, Acormax=1.289, Acor_av=0.936 F test: Probability=1.000, F= 1.210 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06206, wR= 0.07951, Acormin=0.669, Acormax=1.268, Acor_av=0.880 F test: Probability=0.984, F= 1.110 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04995, wR= 0.06754, Acormin=0.624, Acormax=1.293, Acor_av=0.862 F test: Probability=1.000, F= 1.537 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06341, wR= 0.08150, Acormin=0.753, Acormax=1.296, Acor_av=0.935 F test: Probability=0.000, F= 0.619 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05950, wR= 0.07700, Acormin=0.649, Acormax=1.287, Acor_av=0.871 F test: Probability=0.000, F= 0.702 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04852, wR= 0.06521, Acormin=0.607, Acormax=1.309, Acor_av=0.865 F test: Probability=0.850, F= 1.052 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04228, wR= 0.05803, Acormin=0.503, Acormax=1.283, Acor_av=0.830 F test: Probability=1.000, F= 1.376 Trying model 10 (ne=8, no=0)... Results: Rint= 0.06049, wR= 0.07836, Acormin=0.732, Acormax=1.298, Acor_av=0.926 F test: Probability=0.000, F= 0.490 Trying model 11 (ne=8, no=1)... Results: Rint= 0.05038, wR= 0.06640, Acormin=0.684, Acormax=1.408, Acor_av=0.919 F test: Probability=0.000, F= 0.705 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04443, wR= 0.05974, Acormin=0.495, Acormax=1.098, Acor_av=0.717 F test: Probability=0.000, F= 0.902 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03756, wR= 0.05304, Acormin=0.456, Acormax=1.177, Acor_av=0.760 F test: Probability=1.000, F= 1.255 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03485, wR= 0.04921, Acormin=0.468, Acormax=1.228, Acor_av=0.781 F test: Probability=0.998, F= 1.151 Final absorption model (ne=8, no=7): Rint= 0.03485, Acormin=0.468, Acormax=1.228, Acor_av=0.781 Combined refinement in use Rint: 0.10896 There are 79 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13789 Using Levenberg-Marquardt: 0.00010 New wR= 0.04310 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10882 with corrections 0.03124 Rint for all data: 0.10896 with corrections 0.03145 5 observations identified as outliers and rejected Cycle 2 wR= 0.03997 Using Levenberg-Marquardt: 0.00001 New wR= 0.03863 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10833 with corrections 0.02830 Rint for all data: 0.10896 with corrections 0.03135 2 observations identified as outliers and rejected Cycle 3 wR= 0.03781 Using Levenberg-Marquardt: 0.00000 New wR= 0.03758 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10832 with corrections 0.02830 Rint for all data: 0.10896 with corrections 0.03126 0 observations identified as outliers and rejected Cycle 4 wR= 0.03758 Using Levenberg-Marquardt: 0.00000 New wR= 0.03748 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10832 with corrections 0.02835 Rint for all data: 0.10896 with corrections 0.03124 0 observations identified as outliers and rejected Cycle 5 wR= 0.03748 Using Levenberg-Marquardt: 0.00000 New wR= 0.03744 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10832 with corrections 0.02840 Rint for all data: 0.10896 with corrections 0.03125 0 observations identified as outliers and rejected Final wR= 0.03744 Final frame scales: Min= 0.8508 Max= 1.1197 Final absorption correction factors: Amin= 0.5739 Amax= 1.3081 PROFFIT INFO: Inet (after scale3 abspack): min=835.9816 max=6250818.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=116.8502 max=49326.0000 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2256 reflections read from tmp file 256 reflections are rejected (255 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 3 2 0 7 2 6 0 85 Initial Chi^2= 0.34951 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.25933 Current error model SIG(F2)^2 = 163.95*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 370.42*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 370.42*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6250818- 1203504 225 1996182.19 78.68 100.00 1148302- 677013 225 901680.46 36.27 100.00 675624- 299455 225 460345.41 37.01 100.00 298620- 176661 225 218453.62 26.44 100.00 176446- 142385 225 159195.57 17.96 100.00 142213- 98185 225 113109.22 12.84 100.00 98170- 78055 225 88544.09 10.61 100.00 77928- 5750 225 45932.08 7.69 88.00 5713- 3172 225 4155.56 2.68 15.11 3172- 836 231 2461.80 2.27 11.26 ------------------------------------------------------------------------------------ 6250818- 836 2256 397951.36 23.19 81.25 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 225 784538.31 53.95 98.22 1.39- 1.12 225 801486.42 40.48 87.56 1.12- 0.96 225 423217.65 25.75 82.67 0.96- 0.88 225 385760.98 21.87 83.56 0.88- 0.81 225 488693.66 24.61 89.78 0.81- 0.73 225 259275.26 15.02 68.00 0.73- 0.71 225 178704.12 11.98 71.11 0.70- 0.65 225 335924.31 17.49 91.11 0.65- 0.62 225 166241.29 10.64 70.67 0.62- 0.58 231 161964.58 10.45 70.13 ------------------------------------------------------------------------------------ 4.82- 0.58 2256 397951.36 23.19 81.25 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 225 784538.31 53.95 98.22 4.82- 1.12 450 793012.37 47.21 92.89 4.82- 0.96 675 669747.46 40.06 89.48 4.82- 0.88 900 598750.84 35.51 88.00 4.82- 0.81 1125 576739.40 33.33 88.36 4.82- 0.73 1350 523828.71 30.28 84.96 4.82- 0.71 1575 474525.20 27.67 82.98 4.82- 0.65 1800 457200.09 26.39 84.00 4.82- 0.62 2025 424871.33 24.64 82.52 4.82- 0.58 2256 397951.36 23.19 81.25 ------------------------------------------------------------------------------------ 4.82- 0.58 2256 397951.36 23.19 81.25 Scale applied to data: s=0.159979 (maximum obs:6250818.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.031; Rsigma 0.028: data 2256 -> merged 110 With outlier rejection... Rint 0.027; Rsigma 0.028: data 2243 -> merged 110 Rejected total: 13, method kkm 11, method Blessing 2 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585969, 4.832027 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 12.20 100.00 122 1.61 - 1.21 10 10 20.50 100.00 205 1.17 - 1.01 10 10 26.60 100.00 266 0.99 - 0.89 10 10 25.80 100.00 258 0.88 - 0.81 10 10 25.40 100.00 254 0.81 - 0.74 10 10 21.60 100.00 216 0.73 - 0.71 10 10 24.30 100.00 243 0.70 - 0.66 10 10 20.00 100.00 200 0.66 - 0.64 10 10 18.60 100.00 186 0.63 - 0.60 10 10 18.20 100.00 182 --------------------------------------------------------------- 5.92 - 0.60 100 100 21.32 100.00 2132 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 14:53:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918594 5.917917 5.916339 60.0386 90.0649 60.0109 2078 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1024 1119 1021 1042 1582 1388 1395 2078 N (int>3sigma) = 0 902 1119 899 915 1460 1230 1220 1824 Mean intensity = 0.0 57.2 28.0 57.1 62.5 46.8 67.8 65.9 65.5 Mean int/sigma = 0.0 27.2 24.1 26.6 27.5 25.9 29.5 29.0 28.6 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.918 119.96 90.05 119.96 Niggli form: a.a = 34.989 b.b = 35.003 c.c = 35.022 b.c = -17.486 a.c = -0.029 a.b = -17.478 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.050 CUBIC F-lattice R(int) = 0.175 [ 1925] Vol = 586.2 Cell: 8.364 8.373 8.371 90.01 89.97 90.02 Volume: 586.22 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.047 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 1652] Vol = 439.7 Cell: 5.916 5.915 14.501 89.97 90.05 119.96 Volume: 439.67 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.047 RHOMBOHEDRAL R-lattice R(int) = 0.152 [ 522] Vol = 439.7 Trigonal Cell: 5.916 5.915 14.501 89.97 90.05 119.96 Volume: 439.67 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.053 TETRAGONAL I-lattice R(int) = 0.151 [ 1683] Vol = 293.1 Cell: 5.919 5.921 8.364 89.97 90.00 90.02 Volume: 293.11 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.043 TETRAGONAL I-lattice R(int) = 0.151 [ 1683] Vol = 293.1 Cell: 5.919 5.921 8.364 89.97 90.00 90.02 Volume: 293.11 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.038 ORTHORHOMBIC I-lattice R(int) = 0.150 [ 1632] Vol = 293.1 Cell: 5.919 8.364 5.921 89.97 89.98 90.00 Volume: 293.11 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.014 MONOCLINIC I-lattice R(int) = 0.144 [ 1313] Vol = 293.1 Cell: 8.364 5.919 5.921 90.02 90.03 90.00 Volume: 293.11 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.034 MONOCLINIC I-lattice R(int) = 0.136 [ 1319] Vol = 293.1 Cell: 5.918 5.915 8.373 89.99 90.02 89.95 Volume: 293.11 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.028 MONOCLINIC C-lattice R(int) = 0.130 [ 1335] Vol = 293.1 Cell: 8.364 8.373 5.915 89.99 134.96 90.02 Volume: 293.11 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.112 [ 823] Vol = 146.6 Cell: 5.915 5.916 5.918 119.96 90.05 119.96 Volume: 146.56 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1119 0 1388 1388 2078 N (int>3sigma) = 0 0 0 0 1119 0 1216 1230 1824 Mean intensity = 0.0 0.0 0.0 0.0 28.0 0.0 67.5 67.8 65.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 29.3 29.5 28.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 148 487 N I>3s 20 20 94 487 0.7 0.7 0.7 32.9 5.7 5.7 3.8 30.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 1796 Fd-3m 1 1 227 C N N N N 37 2284 0.177 1834 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363821 8.373300 8.370721 90.0131 89.9736 90.0218 ZERR 1.00 0.000297 0.001715 0.003807 0.0023 0.0125 0.0017 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4828365- 607363 504 496 27 18.4 1331546.77 54.12 0.024 0.026 579956- 137077 660 657 27 24.3 241388.71 25.28 0.032 0.039 118211- 41245 566 566 27 21.0 87934.29 10.64 0.044 0.057 11607- 1988 526 524 29 18.1 3943.76 2.72 0.155 0.207 ------------------------------------------------------------------------------------------- 4828365- 1988 2256 2243 110 20.4 388264.34 22.69 0.027 0.030 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 557 545 27 20.2 683509.82 42.00 0.024 0.025 0.016 1.01-0.78 674 673 27 24.9 381365.21 20.88 0.022 0.027 0.029 0.78-0.65 620 620 29 21.4 269518.09 14.94 0.032 0.038 0.042 0.65-0.59 405 405 27 15.0 184207.58 11.59 0.048 0.051 0.058 ------------------------------------------------------------------------------------------------------ inf-0.59 2256 2243 110 20.4 388264.34 22.69 0.027 0.030 0.028 inf-0.60 2143 2130 99 21.5 402060.46 23.39 0.026 0.029 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 545 27 27 100.0 20.2 683509.82 197.69 0.024 0.004 1.01-0.78 673 27 27 100.0 24.9 381365.21 108.12 0.022 0.006 0.78-0.65 620 29 29 100.0 21.4 269518.09 73.45 0.032 0.010 0.65-0.59 405 27 27 100.0 15.0 184207.58 52.45 0.048 0.019 -------------------------------------------------------------------------------------------- inf-0.59 2243 110 110 100.0 20.4 388264.34 110.25 0.027 0.007 inf-0.60 2130 99 99 100.0 21.5 402060.46 114.07 0.026 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:00:50 2018) ID: 2932; threads 39; handles 878; mem 519172.00 (1237700.00)kB; time: 1w 5d 0h 6m 20s MEMORY INFO: Memory PF:0.0, Ph:226.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.0,peak PF: 697.1, WS: 298.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:226.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.8,peak PF: 697.1, WS: 299.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:00:50 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) 5.91502 ( 0.00080 ) 5.91640 ( 0.00080 ) 5.92265 ( 0.00062 ) 60.05206 ( 0.01254 ) 89.98756 ( 0.00968 ) 60.01743 ( 0.01417 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:00:50 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021552 -0.014370 0.007203 ( 0.000003 0.000003 0.000002 ) -0.014370 0.028721 -0.014364 ( 0.000003 0.000004 0.000002 ) 0.007203 -0.014364 0.021557 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(13) 89.988(10) 60.017(14) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb PROFFITPEAK info: 1315 peaks in the peak location table UB fit with 578 obs out of 613 (total:613,skipped:0) (94.29%) UB - matrix: -0.069837 0.031221 0.088950 ( 0.000049 0.000078 0.000058 ) -0.068702 -0.065629 -0.010017 ( 0.000047 0.000074 0.000055 ) 0.109014 -0.153006 0.116399 ( 0.000062 0.000098 0.000073 ) M - matrix: 0.021481 -0.014351 0.007165 ( 0.000016 0.000016 0.000013 ) -0.014351 0.028693 -0.014375 ( 0.000016 0.000032 0.000018 ) 0.007165 -0.014375 0.021561 ( 0.000013 0.000018 0.000020 ) unit cell: 5.931(4) 5.930(4) 5.919(3) 59.93(6) 89.90(5) 59.92(7) V = 147.00(13) UB fit with 578 obs out of 613 (total:613,skipped:0) (94.29%) UB - matrix: -0.069837 0.031221 0.088950 ( 0.000049 0.000078 0.000058 ) -0.068702 -0.065629 -0.010017 ( 0.000047 0.000074 0.000055 ) 0.109014 -0.153006 0.116399 ( 0.000062 0.000098 0.000073 ) M - matrix: 0.021481 -0.014351 0.007165 ( 0.000016 0.000016 0.000013 ) -0.014351 0.028693 -0.014375 ( 0.000016 0.000032 0.000018 ) 0.007165 -0.014375 0.021561 ( 0.000013 0.000018 0.000020 ) unit cell: 5.931(4) 5.930(4) 5.919(3) 59.93(6) 89.90(5) 59.92(7) V = 147.00(13) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.069913 0.031200 0.088854 ( 0.000046 0.000073 0.000054 ) -0.068732 -0.065520 -0.010006 ( 0.000043 0.000070 0.000051 ) 0.108773 -0.152877 0.116290 ( 0.000066 0.000106 0.000078 ) M - matrix: 0.021443 -0.014307 0.007125 ( 0.000017 0.000017 0.000013 ) -0.014307 0.028638 -0.014350 ( 0.000017 0.000034 0.000019 ) 0.007125 -0.014350 0.021518 ( 0.000013 0.000019 0.000020 ) UB fit with 573 obs out of 613 (total:613,skipped:0) (93.47%) unit cell: 5.932(4) 5.935(4) 5.926(3) 59.88(6) 89.82(5) 59.94(6) V = 147.34(13) UB fit with 573 obs out of 613 (total:613,skipped:0) (93.47%) UB - matrix: -0.069913 0.031200 0.088854 ( 0.000046 0.000073 0.000054 ) -0.068732 -0.065520 -0.010006 ( 0.000043 0.000070 0.000051 ) 0.108773 -0.152877 0.116290 ( 0.000066 0.000106 0.000078 ) M - matrix: 0.021443 -0.014307 0.007125 ( 0.000017 0.000017 0.000013 ) -0.014307 0.028638 -0.014350 ( 0.000017 0.000034 0.000019 ) 0.007125 -0.014350 0.021519 ( 0.000013 0.000019 0.000020 ) unit cell: 5.932(4) 5.935(4) 5.926(3) 59.88(6) 89.82(5) 59.94(6) V = 147.34(13) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.069945 0.031201 0.088849 ( 0.000046 0.000073 0.000054 ) -0.068745 -0.065511 -0.010031 ( 0.000044 0.000070 0.000051 ) 0.108761 -0.152869 0.116270 ( 0.000066 0.000106 0.000078 ) M - matrix: 0.021447 -0.014305 0.007121 ( 0.000017 0.000017 0.000013 ) -0.014305 0.028634 -0.014345 ( 0.000017 0.000034 0.000019 ) 0.007121 -0.014345 0.021513 ( 0.000013 0.000019 0.000020 ) UB fit with 573 obs out of 613 (total:613,skipped:0) (93.47%) unit cell: 5.931(4) 5.935(4) 5.926(3) 59.88(6) 89.82(5) 59.94(6) V = 147.33(13) 613 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Run 4 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 749 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069945 0.031201 0.088849 ( 0.000046 0.000073 0.000054 ) -0.068745 -0.065511 -0.010031 ( 0.000044 0.000070 0.000051 ) 0.108761 -0.152869 0.116270 ( 0.000066 0.000106 0.000078 ) M - matrix: 0.021447 -0.014305 0.007121 ( 0.000017 0.000017 0.000013 ) -0.014305 0.028634 -0.014345 ( 0.000017 0.000034 0.000019 ) 0.007121 -0.014345 0.021513 ( 0.000013 0.000019 0.000020 ) UB fit with 573 obs out of 613 (total:613,skipped:0) (93.47%) unit cell: 5.931(4) 5.935(4) 5.926(3) 59.88(6) 89.82(5) 59.94(6) V = 147.33(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 570 obs out of 613 (total:613,skipped:0) (92.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb 8 of 441 peaks identified as outliers and rejected 433 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 433 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 433 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 43 | 1.038 ( 0.157) | 1.131 ( 0.436) | 1.169 ( 0.828) | 1.41- 1.12 | 43 | 1.046 ( 0.092) | 1.260 ( 0.633) | 1.133 ( 0.663) | 1.12- 0.97 | 43 | 1.027 ( 0.101) | 1.060 ( 0.158) | 0.970 ( 0.341) | 0.97- 0.88 | 43 | 1.028 ( 0.094) | 1.024 ( 0.136) | 1.160 ( 0.437) | 0.88- 0.81 | 43 | 1.038 ( 0.083) | 1.002 ( 0.109) | 1.203 ( 0.509) | 0.81- 0.75 | 43 | 1.043 ( 0.078) | 0.993 ( 0.126) | 1.136 ( 0.452) | 0.75- 0.71 | 43 | 1.021 ( 0.045) | 0.935 ( 0.113) | 1.332 ( 0.529) | 0.71- 0.67 | 43 | 1.000 ( 0.040) | 0.889 ( 0.065) | 1.189 ( 0.477) | 0.67- 0.63 | 43 | 0.969 ( 0.043) | 0.843 ( 0.041) | 1.223 ( 0.487) | 0.62- 0.59 | 46 | 0.945 ( 0.041) | 0.811 ( 0.043) | 1.345 ( 0.517) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 433 | 1.015 ( 0.091) | 0.994 ( 0.291) | 1.187 ( 0.549) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 433 obs out of 433 (total:433,skipped:0) (100.00%) UB - matrix: -0.070175 0.031444 0.088653 ( 0.000016 0.000027 0.000022 ) -0.068856 -0.065688 -0.010224 ( 0.000020 0.000033 0.000027 ) 0.108893 -0.152864 0.116131 ( 0.000017 0.000028 0.000023 ) M - matrix: 0.021524 -0.014329 0.007129 ( 0.000005 0.000005 0.000004 ) -0.014329 0.028671 -0.014293 ( 0.000005 0.000010 0.000006 ) 0.007129 -0.014293 0.021450 ( 0.000004 0.000006 0.000007 ) unit cell: 5.9187(15) 5.9198(16) 5.9263(12) 60.03(2) 89.941(18) 59.99(3) V = 146.93(5) OTKP changes: 433 1 1 1 OTKP changes: 433 1 1 1 OTKP changes: 433 1 1 1 UB - matrix: -0.069902 0.031379 0.088704 ( 0.000015 0.000025 0.000020 ) -0.068761 -0.065707 -0.009997 ( 0.000018 0.000029 0.000023 ) 0.108905 -0.152882 0.116254 ( 0.000017 0.000027 0.000022 ) M - matrix: 0.021475 -0.014325 0.007147 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028675 -0.014333 ( 0.000005 0.000009 0.000005 ) 0.007147 -0.014333 0.021483 ( 0.000004 0.000005 0.000006 ) UB fit with 433 obs out of 433 (total:433,skipped:0) (100.00%) unit cell: 5.9277(14) 5.9252(14) 5.9275(11) 59.97(2) 89.949(16) 59.99(2) V = 147.17(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069902 0.031379 0.088704 ( 0.000015 0.000025 0.000020 ) -0.068761 -0.065707 -0.009997 ( 0.000018 0.000029 0.000023 ) 0.108905 -0.152882 0.116254 ( 0.000017 0.000027 0.000022 ) M - matrix: 0.021475 -0.014325 0.007147 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028675 -0.014333 ( 0.000005 0.000009 0.000005 ) 0.007147 -0.014333 0.021483 ( 0.000004 0.000005 0.000006 ) UB fit with 433 obs out of 433 (total:433,skipped:0) (100.00%) unit cell: 5.9277(14) 5.9252(14) 5.9275(11) 59.97(2) 89.949(16) 59.99(2) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 433 obs out of 433 (total:433,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb 7 of 439 peaks identified as outliers and rejected 432 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 432 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 432 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 43 | 1.034 ( 0.153) | 1.129 ( 0.438) | 1.146 ( 0.783) | 1.41- 1.12 | 43 | 1.043 ( 0.086) | 1.241 ( 0.583) | 1.121 ( 0.658) | 1.12- 0.97 | 43 | 1.023 ( 0.107) | 1.034 ( 0.129) | 0.988 ( 0.348) | 0.97- 0.88 | 43 | 1.034 ( 0.089) | 1.031 ( 0.134) | 1.156 ( 0.428) | 0.88- 0.81 | 43 | 1.039 ( 0.082) | 1.007 ( 0.114) | 1.179 ( 0.511) | 0.81- 0.75 | 43 | 1.036 ( 0.079) | 0.983 ( 0.131) | 1.135 ( 0.434) | 0.74- 0.71 | 43 | 1.022 ( 0.042) | 0.940 ( 0.111) | 1.286 ( 0.534) | 0.71- 0.67 | 43 | 1.000 ( 0.041) | 0.890 ( 0.071) | 1.208 ( 0.470) | 0.67- 0.63 | 43 | 0.971 ( 0.044) | 0.844 ( 0.042) | 1.236 ( 0.488) | 0.63- 0.59 | 45 | 0.946 ( 0.041) | 0.810 ( 0.043) | 1.334 ( 0.521) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 432 | 1.014 ( 0.089) | 0.990 ( 0.277) | 1.180 ( 0.538) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 176 | 1.119 ( 0.116) | 1.233 ( 0.452) | 1.177 ( 0.608) | 13.2-19.0 | 176 | 1.082 ( 0.052) | 1.132 ( 0.247) | 1.218 ( 0.533) | 19.0-23.2 | 176 | 1.070 ( 0.073) | 1.148 ( 0.391) | 1.170 ( 0.506) | 23.2-27.2 | 176 | 1.038 ( 0.080) | 1.073 ( 0.285) | 1.207 ( 0.576) | 27.2-30.8 | 176 | 1.014 ( 0.076) | 1.016 ( 0.263) | 1.198 ( 0.509) | 30.9-33.8 | 176 | 0.986 ( 0.084) | 0.926 ( 0.098) | 1.190 ( 0.514) | 33.8-36.9 | 176 | 0.967 ( 0.077) | 0.902 ( 0.098) | 1.185 ( 0.487) | 36.9-39.7 | 176 | 0.950 ( 0.093) | 0.876 ( 0.142) | 1.173 ( 0.546) | 39.7-42.8 | 176 | 0.929 ( 0.081) | 0.837 ( 0.080) | 1.193 ( 0.515) | 42.8-49.9 | 175 | 0.939 ( 0.081) | 0.816 ( 0.065) | 1.151 ( 0.452) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1759 | 1.009 ( 0.104) | 0.996 ( 0.284) | 1.186 ( 0.527) | Fitted profile normalization line parameters e1 dimension: a=-0.0046 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0016 b=1.03 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3688575 PROFFITPEAK - Finished at Tue Mar 27 15:01:08 2018 PROFFITMAIN - Started at Tue Mar 27 15:01:08 2018 OTKP changes: 1759 2 3 4 OTKP changes: 1759 2 3 4 UB - matrix: -0.070169 0.031104 0.088938 ( 0.000011 0.000012 0.000011 ) -0.068699 -0.065914 -0.010418 ( 0.000012 0.000013 0.000012 ) 0.109151 -0.153012 0.116313 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021557 -0.014356 0.007171 ( 0.000003 0.000002 0.000002 ) -0.014356 0.028725 -0.014344 ( 0.000002 0.000004 0.000002 ) 0.007171 -0.014344 0.021547 ( 0.000002 0.000002 0.000003 ) UB fit with 1759 obs out of 1759 (total:1759,skipped:0) (100.00%) unit cell: 5.9144(7) 5.9137(7) 5.9141(6) 60.043(11) 90.007(9) 60.016(13) V = 146.39(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070040 0.030657 0.088974 ( 0.000029 0.000028 0.000016 ) -0.068253 -0.066142 -0.010489 ( 0.000026 0.000025 0.000015 ) 0.109063 -0.153048 0.115956 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021459 -0.014325 0.007131 ( 0.000008 0.000006 0.000004 ) -0.014325 0.028738 -0.014325 ( 0.000006 0.000008 0.000005 ) 0.007131 -0.014325 0.021472 ( 0.000004 0.000005 0.000004 ) unit cell: 5.9276(14) 5.9137(14) 5.9250(11) 60.01(2) 89.960(18) 60.00(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070325 0.030930 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068403 -0.066125 -0.010686 ( 0.000024 0.000023 0.000013 ) 0.109327 -0.153276 0.116356 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021577 -0.014409 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014409 0.028823 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9163(13) 5.9079(13) 5.9185(10) 60.05(2) 90.069(16) 60.00(2) V = 146.29(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.799) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070325 0.030930 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068403 -0.066125 -0.010686 ( 0.000024 0.000023 0.000013 ) 0.109327 -0.153276 0.116356 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021577 -0.014409 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014409 0.028823 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9163(13) 5.9079(13) 5.9185(10) 60.05(2) 90.069(16) 60.00(2) V = 146.29(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070325 0.030930 0.088799 ( 0.000026 0.000026 0.000015 ) -0.068403 -0.066125 -0.010686 ( 0.000024 0.000023 0.000013 ) 0.109327 -0.153276 0.116356 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021577 -0.014409 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014409 0.028823 -0.014381 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014381 0.021538 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9163(13) 5.9079(13) 5.9185(10) 60.05(2) 90.069(16) 60.00(2) V = 146.29(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031359 0.088642 ( 0.000026 0.000023 0.000028 ) -0.068572 -0.066012 -0.010221 ( 0.000031 0.000027 0.000033 ) 0.108984 -0.152622 0.116241 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021537 -0.014315 0.007128 ( 0.000007 0.000005 0.000005 ) -0.014315 0.028635 -0.014287 ( 0.000005 0.000007 0.000005 ) 0.007128 -0.014287 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(17) 5.9211(17) 5.9219(14) 60.03(3) 89.94(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070357 0.031203 0.088836 ( 0.000023 0.000020 0.000025 ) -0.068778 -0.065856 -0.010352 ( 0.000030 0.000026 0.000032 ) 0.109159 -0.153138 0.116571 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021596 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014398 0.021588 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9099(16) 5.9168(16) 5.9149(12) 59.94(2) 89.948(19) 60.01(3) V = 146.20(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.799) HKL list info: 719 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070357 0.031203 0.088836 ( 0.000023 0.000020 0.000025 ) -0.068778 -0.065856 -0.010352 ( 0.000030 0.000026 0.000032 ) 0.109159 -0.153138 0.116571 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021596 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014398 0.021588 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9099(16) 5.9168(16) 5.9149(12) 59.94(2) 89.948(19) 60.01(3) V = 146.20(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070357 0.031203 0.088836 ( 0.000023 0.000020 0.000025 ) -0.068778 -0.065856 -0.010352 ( 0.000030 0.000026 0.000032 ) 0.109159 -0.153138 0.116571 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021596 -0.014382 0.007186 ( 0.000007 0.000005 0.000005 ) -0.014382 0.028762 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007186 -0.014398 0.021588 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9099(16) 5.9168(16) 5.9149(12) 59.94(2) 89.948(19) 60.01(3) V = 146.20(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) UB - matrix: -0.070170 0.031446 0.088652 ( 0.000016 0.000027 0.000022 ) -0.068854 -0.065707 -0.010215 ( 0.000022 0.000035 0.000029 ) 0.108905 -0.152862 0.116137 ( 0.000017 0.000028 0.000022 ) M - matrix: 0.021525 -0.014330 0.007131 ( 0.000005 0.000005 0.000004 ) -0.014330 0.028673 -0.014294 ( 0.000005 0.000010 0.000006 ) 0.007131 -0.014294 0.021451 ( 0.000004 0.000006 0.000006 ) unit cell: 5.9183(16) 5.9194(16) 5.9262(12) 60.03(2) 89.948(19) 59.99(3) V = 146.92(6) OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 OTKP changes: 432 1 1 1 UB - matrix: -0.070100 0.031424 0.088896 ( 0.000015 0.000025 0.000021 ) -0.068714 -0.066031 -0.009948 ( 0.000019 0.000031 0.000025 ) 0.109193 -0.153117 0.116568 ( 0.000016 0.000026 0.000021 ) M - matrix: 0.021559 -0.014385 0.007180 ( 0.000005 0.000005 0.000004 ) -0.014385 0.028792 -0.014398 ( 0.000005 0.000009 0.000005 ) 0.007180 -0.014398 0.021590 ( 0.000004 0.000005 0.000006 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9166(14) 5.9136(14) 5.9130(11) 59.97(2) 89.948(17) 59.98(2) V = 146.24(5) Run 4 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.799) HKL list info: 741 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070100 0.031424 0.088896 ( 0.000015 0.000025 0.000021 ) -0.068714 -0.066031 -0.009948 ( 0.000019 0.000031 0.000025 ) 0.109193 -0.153117 0.116568 ( 0.000016 0.000026 0.000021 ) M - matrix: 0.021559 -0.014385 0.007180 ( 0.000005 0.000005 0.000004 ) -0.014385 0.028792 -0.014398 ( 0.000005 0.000009 0.000005 ) 0.007180 -0.014398 0.021590 ( 0.000004 0.000005 0.000006 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9166(14) 5.9136(14) 5.9130(11) 59.97(2) 89.948(17) 59.98(2) V = 146.24(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070100 0.031424 0.088896 ( 0.000015 0.000025 0.000021 ) -0.068714 -0.066031 -0.009948 ( 0.000019 0.000031 0.000025 ) 0.109193 -0.153117 0.116568 ( 0.000016 0.000026 0.000021 ) M - matrix: 0.021559 -0.014385 0.007180 ( 0.000005 0.000005 0.000004 ) -0.014385 0.028792 -0.014398 ( 0.000005 0.000009 0.000005 ) 0.007180 -0.014398 0.021590 ( 0.000004 0.000005 0.000006 ) UB fit with 432 obs out of 432 (total:432,skipped:0) (100.00%) unit cell: 5.9166(14) 5.9136(14) 5.9130(11) 59.97(2) 89.948(17) 59.98(2) V = 146.24(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070043 0.031076 0.088896 ( 0.000012 0.000013 0.000012 ) -0.068678 -0.065803 -0.010467 ( 0.000014 0.000015 0.000014 ) 0.109203 -0.153060 0.116402 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021548 -0.014372 0.007204 ( 0.000003 0.000003 0.000002 ) -0.014372 0.028723 -0.014365 ( 0.000003 0.000004 0.000002 ) 0.007204 -0.014365 0.021561 ( 0.000002 0.000002 0.000003 ) UB fit with 1759 obs out of 1759 (total:1759,skipped:0) (100.00%) unit cell: 5.9197(8) 5.9180(8) 5.9156(6) 60.042(13) 90.063(10) 60.003(14) V = 146.56(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 59 reflections under beam stop or inside a detector rejection region 17 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof 2394 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:01:13 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.799) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.799) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.799) PROFFIT INFO: signal sum: min=249.0000 max=20845746.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2959208.2177 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4734733.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47756.1563 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=251.33 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 12 89 223 483 539 944 1576 2183 2394 Percent 0.0 0.0 0.5 3.7 9.3 20.2 22.5 39.4 65.8 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2394 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2394 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4734734- 1228602 239 1983350.98 121.62 100.00 1225306- 713211 239 932742.37 107.03 100.00 712347- 283452 239 462766.01 97.77 100.00 282068- 180602 239 217545.80 74.43 100.00 180524- 136011 239 159227.00 52.25 100.00 135852- 101977 239 116151.52 37.28 100.00 101974- 79302 239 90739.16 30.21 100.00 79036- 5927 239 45556.04 20.74 100.00 5918- 3253 239 4277.15 5.56 97.49 3246- 924 243 2471.92 4.05 65.84 ------------------------------------------------------------------------------------ 4734734- 924 2394 400816.11 55.01 96.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 239 738448.66 88.50 99.16 1.32- 1.05 239 587212.00 68.00 97.49 1.05- 0.92 239 488672.36 62.59 97.91 0.92- 0.82 239 356306.11 53.55 96.23 0.82- 0.74 239 438024.62 58.21 97.07 0.74- 0.67 239 392287.53 56.52 96.65 0.67- 0.62 239 246432.11 42.58 96.23 0.62- 0.56 239 329257.53 48.30 93.31 0.56- 0.51 239 236565.99 39.11 93.72 0.51- 0.40 243 198342.87 33.09 95.06 ------------------------------------------------------------------------------------ 5.26- 0.40 2394 400816.11 55.01 96.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:01:13 2018 Sorting 2394 observations 280 unique observations with > 7.00 F2/sig(F2) 2394 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 99 413 Total number of frames 413 Maximum number of 280 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2394 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 49 209 Total number of frames 209 1931 observations > 7.00 F2/sig(F2) 1931 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 49 209 Total number of frames 209 Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 1931 removed 39 = 1892, unique = 262) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1892 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 49 209 Total number of frames 209 262 unique data precomputed (should be 262) 262 unique data with 1892 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.2 (Out of 1892 removed 0 = 1892, unique = 262) 262 unique data precomputed (should be 262) 262 unique data with 1892 observations RMS deviation of equivalent data = 0.71356 Rint = 0.68593 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66297, wR= 3.57505 Trying model 1 (ne=2, no=0)... Results: Rint= 0.70205, wR= 2.80569, Acormin=-0.017, Acormax=2.010, Acor_av=0.717 F test: Probability=0.000, F= 0.889 Trying model 2 (ne=2, no=1)... Results: Rint= 0.86125, wR= 2.62446, Acormin=-0.560, Acormax=1.758, Acor_av=0.411 F test: Probability=0.000, F= 0.590 Trying model 3 (ne=4, no=0)... Results: Rint= 0.73326, wR= 2.36959, Acormin=-0.116, Acormax=2.325, Acor_av=0.597 F test: Probability=0.000, F= 0.810 Trying model 4 (ne=4, no=1)... Results: Rint= 0.89706, wR= 2.24510, Acormin=-0.410, Acormax=1.732, Acor_av=0.331 F test: Probability=0.000, F= 0.540 Trying model 5 (ne=4, no=3)... Results: Rint= 0.94967, wR= 2.01453, Acormin=-0.999, Acormax=1.699, Acor_av=0.183 F test: Probability=0.000, F= 0.480 Trying model 6 (ne=6, no=0)... Results: Rint= 0.77454, wR= 2.39718, Acormin=-0.295, Acormax=2.784, Acor_av=0.489 F test: Probability=0.000, F= 0.720 Trying model 7 (ne=6, no=1)... Results: Rint= 0.92290, wR= 2.28364, Acormin=-0.594, Acormax=2.093, Acor_av=0.253 F test: Probability=0.000, F= 0.506 Trying model 8 (ne=6, no=3)... Results: Rint= 0.96300, wR= 2.18377, Acormin=-1.315, Acormax=1.869, Acor_av=0.133 F test: Probability=0.000, F= 0.463 Trying model 9 (ne=6, no=5)... Results: Rint= 0.95603, wR= 2.28371, Acormin=-1.390, Acormax=1.716, Acor_av=0.115 F test: Probability=0.000, F= 0.467 Trying model 10 (ne=8, no=0)... Results: Rint= 0.86506, wR= 2.24834, Acormin=-0.667, Acormax=2.894, Acor_av=0.352 F test: Probability=0.000, F= 0.571 Trying model 11 (ne=8, no=1)... Results: Rint= 0.98464, wR= 1.83274, Acormin=-1.341, Acormax=1.529, Acor_av=0.098 F test: Probability=0.000, F= 0.440 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98998, wR= 1.54222, Acormin=-0.043, Acormax=0.076, Acor_av=0.001 F test: Probability=0.000, F= 0.433 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99823, wR= 1.55568, Acormin=-0.043, Acormax=0.094, Acor_av=0.002 F test: Probability=0.000, F= 0.423 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00556, wR= 1.66885, Acormin=-0.041, Acormax=0.083, Acor_av=0.002 F test: Probability=0.000, F= 0.413 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.85149 There are 209 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 213 pars with 22791 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71356 Using Levenberg-Marquardt: 0.00010 New wR= 0.69121 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68593 with corrections 0.65758 Rint for all data: 0.85149 with corrections 0.83057 12 observations identified as outliers and rejected Cycle 2 wR= 0.66524 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.66373 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66297 with corrections 0.64067 Rint for all data: 0.85149 with corrections 0.83649 11 observations identified as outliers and rejected Cycle 3 wR= 0.64146 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63959 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65079 with corrections 0.62969 Rint for all data: 0.85149 with corrections 0.83867 11 observations identified as outliers and rejected Cycle 4 wR= 0.61654 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61527 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64324 with corrections 0.62751 Rint for all data: 0.85149 with corrections 0.84041 10 observations identified as outliers and rejected Cycle 5 wR= 0.59414 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59058 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64110 with corrections 0.62448 Rint for all data: 0.85149 with corrections 0.83885 3 observations identified as outliers and rejected Final wR= 0.59058 Final frame scales: Min= 0.5399 Max= 4.3458 Final absorption correction factors: Amin= 0.3955 Amax= 1.3671 PROFFIT INFO: Inet (after scale3 abspack): min=767.2999 max=6099369.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=136.4906 max=74470.5625 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2394 reflections read from tmp file 1828 reflections are rejected (1750 as outliers, 78 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 88 40 27 12 8 4 2 0 1 Initial Chi^2= 0.56676 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.81048 Current error model SIG(F2)^2 = 196.59*I_RAW + 0.00*I_BACK+(0.03524*)^2 Cycle 2, Chi^2= 1.00258 Current error model SIG(F2)^2 = 188.27*I_RAW + 0.00*I_BACK+(0.02300*)^2 Cycle 3, Chi^2= 1.00229 Current error model SIG(F2)^2 = 197.12*I_RAW + 0.00*I_BACK+(0.02043*)^2 Cycle 4, Chi^2= 0.99987 Current error model SIG(F2)^2 = 197.07*I_RAW + 0.00*I_BACK+(0.02061*)^2 Cycle 5, Chi^2= 1.00002 Current error model SIG(F2)^2 = 197.11*I_RAW + 0.00*I_BACK+(0.02059*)^2 Final Chi^2= 1.00002 Final error model SIG(F2)^2 = 197.11*I_RAW + 0.00*I_BACK+(0.02059*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6099369- 1226293 239 1995075.57 94.57 100.00 1225492- 653000 239 895773.39 50.33 100.00 652663- 269030 239 429189.58 45.26 100.00 268333- 177019 239 216295.18 32.86 100.00 176734- 136202 239 153912.88 22.56 100.00 135929- 99544 239 118140.45 18.63 100.00 99539- 69180 239 84191.58 14.15 100.00 69022- 6206 239 40154.80 10.41 94.98 6187- 3032 239 4179.74 3.54 65.27 3030- 767 243 2259.40 2.80 32.92 ------------------------------------------------------------------------------------ 6099369- 767 2394 393262.86 29.47 89.22 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 239 822341.47 61.50 96.65 1.32- 1.05 239 594941.18 43.81 95.40 1.05- 0.92 239 512193.22 34.16 92.89 0.92- 0.82 239 355276.41 27.77 85.36 0.82- 0.74 239 435206.00 27.49 91.21 0.74- 0.67 239 366557.89 26.29 88.28 0.67- 0.62 239 224441.23 19.86 85.36 0.62- 0.56 239 287794.62 21.09 84.10 0.56- 0.51 239 192776.76 17.99 84.94 0.51- 0.40 243 145250.64 14.97 88.07 ------------------------------------------------------------------------------------ 5.26- 0.40 2394 393262.86 29.47 89.22 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 239 822341.47 61.50 96.65 5.26- 1.05 478 708641.32 52.65 96.03 5.26- 0.92 717 643158.62 46.49 94.98 5.26- 0.82 956 571188.07 41.81 92.57 5.26- 0.74 1195 543991.65 38.94 92.30 5.26- 0.67 1434 514419.36 36.84 91.63 5.26- 0.62 1673 472993.91 34.41 90.74 5.26- 0.56 1912 449844.00 32.75 89.91 5.26- 0.51 2151 421280.98 31.11 89.35 5.26- 0.40 2394 393262.86 29.47 89.22 ------------------------------------------------------------------------------------ 5.26- 0.40 2394 393262.86 29.47 89.22 Scale applied to data: s=0.163951 (maximum obs:6099369.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.839; Rsigma 0.022: data 2394 -> merged 313 With outlier rejection... Rint 0.762; Rsigma 0.023: data 2217 -> merged 313 Rejected total: 177, method kkm 165, method Blessing 12 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404371, 5.272350 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 10.40 100.00 156 1.46 - 1.12 15 15 16.93 100.00 254 1.08 - 0.96 15 15 14.87 100.00 223 0.96 - 0.86 15 15 13.60 100.00 204 0.86 - 0.79 15 15 11.87 100.00 178 0.79 - 0.73 15 15 10.33 100.00 155 0.73 - 0.69 15 15 9.13 100.00 137 0.69 - 0.65 15 15 9.47 100.00 142 0.65 - 0.63 15 15 5.53 100.00 83 0.63 - 0.60 21 21 6.14 100.00 129 --------------------------------------------------------------- 5.92 - 0.60 156 156 10.65 100.00 1661 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:01:14 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919749 5.918019 5.915550 60.0420 90.0632 60.0026 2217 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1093 1188 1089 1122 1685 1490 1478 2217 N (int>3sigma) = 0 970 1188 966 1026 1562 1343 1308 1981 Mean intensity = 0.0 53.5 26.5 53.3 58.3 43.9 63.8 61.7 61.4 Mean int/sigma = 0.0 28.3 24.9 27.8 28.2 26.9 29.5 28.9 28.9 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.918 119.96 90.04 119.96 Niggli form: a.a = 34.989 b.b = 34.994 c.c = 35.023 b.c = -17.482 a.c = -0.026 a.b = -17.473 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.059 CUBIC F-lattice R(int) = 0.195 [ 2064] Vol = 586.2 Cell: 8.364 8.373 8.370 90.01 89.97 90.04 Volume: 586.24 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.052 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 1789] Vol = 439.7 Cell: 5.916 5.915 14.503 89.98 90.05 119.96 Volume: 439.68 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.052 RHOMBOHEDRAL R-lattice R(int) = 0.161 [ 559] Vol = 439.7 Trigonal Cell: 5.916 5.915 14.503 89.98 90.05 119.96 Volume: 439.68 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.081 TETRAGONAL I-lattice R(int) = 0.158 [ 1821] Vol = 293.1 Cell: 5.919 5.921 8.364 89.95 90.01 90.02 Volume: 293.12 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.158 [ 1821] Vol = 293.1 Cell: 5.919 5.921 8.364 89.95 90.01 90.02 Volume: 293.12 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.040 ORTHORHOMBIC I-lattice R(int) = 0.161 [ 1770] Vol = 293.1 Cell: 5.919 8.364 5.921 89.95 89.98 89.99 Volume: 293.12 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.154 [ 1446] Vol = 293.1 Cell: 8.364 5.919 5.921 90.02 90.05 89.99 Volume: 293.12 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.033 MONOCLINIC I-lattice R(int) = 0.150 [ 1459] Vol = 293.1 Cell: 5.918 5.915 8.373 89.98 90.04 89.96 Volume: 293.12 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.051 MONOCLINIC C-lattice R(int) = 0.134 [ 1472] Vol = 293.1 Cell: 8.364 8.373 5.915 89.98 134.96 90.04 Volume: 293.12 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.117 [ 941] Vol = 146.6 Cell: 5.915 5.916 5.918 119.96 90.04 119.96 Volume: 146.56 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1188 0 1479 1490 2217 N (int>3sigma) = 0 0 0 0 1188 0 1323 1343 1981 Mean intensity = 0.0 0.0 0.0 0.0 26.5 0.0 62.9 63.8 61.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.9 0.0 29.5 29.5 28.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 162 514 N I>3s 18 18 106 514 0.7 0.7 0.6 31.6 5.8 5.8 3.7 31.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.195 1921 Fd-3m 1 1 227 C N N N N 37 2284 0.196 1959 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364204 8.373435 8.370369 90.0138 89.9718 90.0407 ZERR 1.00 0.000301 0.001719 0.003819 0.0022 0.0127 0.0017 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3300850- 648594 395 365 31 11.8 991311.10 51.32 0.662 0.631 645892- 475169 327 319 31 10.3 542692.79 42.59 0.886 0.819 471617- 364591 223 212 31 6.8 395804.14 30.01 0.889 0.818 359871- 294870 324 309 31 10.0 311270.92 28.17 0.950 1.081 294713- 220307 221 191 31 6.2 192688.60 19.87 0.839 0.852 218307- 167051 254 221 31 7.1 146951.67 21.77 0.609 0.680 160755- 93902 257 240 31 7.7 102437.88 16.42 0.529 0.524 92621- 67848 160 146 31 4.7 81459.69 14.06 0.412 0.242 66715- 47689 127 115 31 3.7 58654.05 11.76 0.452 0.290 46937- 1740 106 99 34 2.9 23425.80 6.30 0.731 0.676 ------------------------------------------------------------------------------------------- 3300850- 1740 2394 2217 313 7.1 374318.07 28.85 0.762 0.740 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 466 432 31 13.9 687917.56 52.12 0.738 0.774 0.015 1.05-0.83 438 428 31 13.8 441070.57 31.46 0.897 1.044 0.021 0.83-0.72 367 350 33 10.6 377344.55 26.01 0.742 0.769 0.027 0.72-0.65 296 276 32 8.6 261255.05 22.32 0.786 0.782 0.029 0.64-0.60 225 194 31 6.3 242679.35 19.71 0.758 0.735 0.032 0.59-0.56 195 180 35 5.1 171739.51 16.57 0.607 0.565 0.039 0.55-0.52 150 135 31 4.4 237768.74 20.09 0.611 0.613 0.034 0.51-0.49 120 103 31 3.3 134801.16 14.62 0.602 0.519 0.043 0.49-0.45 83 72 31 2.3 149808.86 14.97 0.372 0.264 0.042 0.45-0.40 54 47 27 1.7 105641.27 13.12 0.264 0.264 0.050 ------------------------------------------------------------------------------------------------------ inf-0.40 2394 2217 313 7.1 374318.07 28.85 0.762 0.740 0.023 inf-0.60 1771 1661 156 10.6 441720.06 32.92 0.786 0.829 0.021 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 432 31 31 100.0 13.9 687917.56 228.67 0.738 0.005 1.05-0.83 428 31 31 100.0 13.8 441070.57 142.97 0.897 0.008 0.83-0.72 350 33 33 100.0 10.6 377344.55 105.77 0.742 0.011 0.72-0.65 276 32 32 100.0 8.6 261255.05 83.23 0.786 0.014 0.64-0.60 194 31 31 100.0 6.3 242679.35 65.57 0.758 0.017 0.59-0.56 180 38 35 92.1 5.1 171739.51 47.78 0.607 0.019 0.55-0.52 135 37 31 83.8 4.4 237768.74 53.35 0.611 0.018 0.51-0.49 103 43 31 72.1 3.3 134801.16 32.69 0.602 0.029 0.49-0.45 72 61 31 50.8 2.3 149808.86 26.54 0.372 0.029 0.45-0.40 47 124 27 21.8 1.7 105641.27 17.95 0.264 0.037 -------------------------------------------------------------------------------------------- inf-0.40 2217 464 313 67.5 7.1 374318.07 114.84 0.762 0.013 inf-0.60 1661 156 156 100.0 10.6 441720.06 139.36 0.786 0.009 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: -0.024964 -0.079469 -0.015538 ( 0.000007 0.000007 0.000006 ) 0.072475 -0.029105 0.032901 ( 0.000008 0.000008 0.000007 ) -0.036272 -0.003599 0.076530 ( 0.000005 0.000006 0.000005 ) M - matrix: 0.007191 0.000005 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000005 0.007175 0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000002 0.007181 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024964 -0.079469 -0.015538 ( 0.000007 0.000007 0.000006 ) 0.072475 -0.029105 0.032901 ( 0.000008 0.000008 0.000007 ) -0.036272 -0.003599 0.076530 ( 0.000005 0.000006 0.000005 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3642(7) 8.3735(7) 8.3704(6) 90.014(6) 89.972(6) 90.040(7) V = 586.24(8) unit cell: 8.3694(2) 8.3694(2) 8.3694(2) 90.0 90.0 90.0 V = 586.24(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.799) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.799) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.799) PROFFIT INFO: signal sum: min=249.0000 max=20845746.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2959208.2177 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4734733.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47756.1563 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=251.33 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 24 178 446 966 1078 1888 3152 4366 4788 Percent 0.0 0.0 0.5 3.7 9.3 20.2 22.5 39.4 65.8 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2394 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2394 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4734734- 1228602 239 1983350.98 121.62 100.00 1225306- 713211 239 932742.37 107.03 100.00 712347- 283452 239 462766.01 97.77 100.00 282068- 180602 239 217545.80 74.43 100.00 180524- 136011 239 159227.00 52.25 100.00 135852- 101977 239 116151.52 37.28 100.00 101974- 79302 239 90739.16 30.21 100.00 79036- 5927 239 45556.04 20.74 100.00 5918- 3253 239 4277.15 5.56 97.49 3246- 924 243 2471.92 4.05 65.84 ------------------------------------------------------------------------------------ 4734734- 924 2394 400816.11 55.01 96.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 239 771920.68 94.44 100.00 1.39- 1.12 239 817442.52 67.04 100.00 1.09- 0.96 239 392340.18 68.02 97.49 0.96- 0.85 239 398689.86 63.38 96.65 0.85- 0.81 239 489347.58 71.11 99.58 0.81- 0.73 239 266965.74 42.59 99.58 0.73- 0.70 239 199412.77 35.31 86.61 0.70- 0.65 239 334749.44 49.43 94.98 0.65- 0.62 239 174662.31 30.00 90.79 0.62- 0.58 243 166550.79 29.20 97.12 ------------------------------------------------------------------------------------ 4.82- 0.58 2394 400816.11 55.01 96.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:01:14 2018 Sorting 2394 observations 85 unique observations with > 7.00 F2/sig(F2) 2394 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 99 413 Total number of frames 413 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2394 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 19 84 Total number of frames 84 1931 observations > 7.00 F2/sig(F2) 1931 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 19 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 20.7 (Out of 1931 removed 3 = 1928, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1928 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 19 84 Total number of frames 84 93 unique data precomputed (should be 93) 93 unique data with 1928 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.7 (Out of 1928 removed 0 = 1928, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 1928 observations RMS deviation of equivalent data = 0.13717 Rint = 0.10657 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10563, wR= 0.13597 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07732, wR= 0.09541, Acormin=0.808, Acormax=1.244, Acor_av=0.977 F test: Probability=1.000, F= 1.861 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07066, wR= 0.08831, Acormin=0.743, Acormax=1.298, Acor_av=0.946 F test: Probability=1.000, F= 1.195 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06484, wR= 0.08293, Acormin=0.746, Acormax=1.295, Acor_av=0.939 F test: Probability=1.000, F= 1.184 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06099, wR= 0.07882, Acormin=0.675, Acormax=1.272, Acor_av=0.881 F test: Probability=0.995, F= 1.128 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04862, wR= 0.06623, Acormin=0.634, Acormax=1.306, Acor_av=0.869 F test: Probability=1.000, F= 1.567 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06279, wR= 0.08051, Acormin=0.751, Acormax=1.295, Acor_av=0.935 F test: Probability=0.000, F= 0.599 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05830, wR= 0.07640, Acormin=0.670, Acormax=1.285, Acor_av=0.871 F test: Probability=0.000, F= 0.693 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04715, wR= 0.06376, Acormin=0.617, Acormax=1.318, Acor_av=0.870 F test: Probability=0.874, F= 1.056 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04155, wR= 0.05706, Acormin=0.525, Acormax=1.288, Acor_av=0.834 F test: Probability=1.000, F= 1.351 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05936, wR= 0.07688, Acormin=0.702, Acormax=1.301, Acor_av=0.924 F test: Probability=0.000, F= 0.491 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04966, wR= 0.06524, Acormin=0.680, Acormax=1.410, Acor_av=0.917 F test: Probability=0.000, F= 0.700 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04317, wR= 0.05837, Acormin=0.504, Acormax=1.116, Acor_av=0.726 F test: Probability=0.000, F= 0.923 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03724, wR= 0.05220, Acormin=0.467, Acormax=1.189, Acor_av=0.766 F test: Probability=1.000, F= 1.233 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03471, wR= 0.04858, Acormin=0.482, Acormax=1.242, Acor_av=0.786 F test: Probability=0.997, F= 1.141 Final absorption model (ne=8, no=7): Rint= 0.03471, Acormin=0.482, Acormax=1.242, Acor_av=0.786 Combined refinement in use Rint: 0.10671 There are 84 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13717 Using Levenberg-Marquardt: 0.00010 New wR= 0.04276 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10657 with corrections 0.03085 Rint for all data: 0.10671 with corrections 0.03106 3 observations identified as outliers and rejected Cycle 2 wR= 0.03986 Using Levenberg-Marquardt: 0.00001 New wR= 0.03859 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10620 with corrections 0.02809 Rint for all data: 0.10671 with corrections 0.03106 2 observations identified as outliers and rejected Cycle 3 wR= 0.03761 Using Levenberg-Marquardt: 0.00000 New wR= 0.03699 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10555 with corrections 0.02730 Rint for all data: 0.10671 with corrections 0.03114 0 observations identified as outliers and rejected Cycle 4 wR= 0.03699 Using Levenberg-Marquardt: 0.00000 New wR= 0.03686 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10555 with corrections 0.02724 Rint for all data: 0.10671 with corrections 0.03103 0 observations identified as outliers and rejected Cycle 5 wR= 0.03686 Using Levenberg-Marquardt: 0.00000 New wR= 0.03678 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10555 with corrections 0.02721 Rint for all data: 0.10671 with corrections 0.03096 0 observations identified as outliers and rejected Final wR= 0.03678 Final frame scales: Min= 0.8560 Max= 1.1504 Final absorption correction factors: Amin= 0.5789 Amax= 1.3046 PROFFIT INFO: Inet (after scale3 abspack): min=821.1054 max=6340233.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=137.7098 max=49657.4609 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2394 reflections read from tmp file 263 reflections are rejected (261 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 1 2 5 4 2 3 85 Initial Chi^2= 0.33792 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.98955 Current error model SIG(F2)^2 = 160.68*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 319.69*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 319.69*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6340233- 1246864 239 2013698.97 85.34 100.00 1236548- 679994 239 907261.31 39.09 100.00 679893- 299427 239 460287.20 39.92 100.00 299165- 176927 239 218651.73 28.50 100.00 176795- 143956 239 160058.21 19.26 100.00 143586- 98410 239 113255.89 13.83 100.00 98305- 78101 239 88503.43 11.37 100.00 78076- 5637 239 45794.55 8.22 90.79 5590- 3183 239 4136.00 2.89 20.50 3178- 821 243 2489.00 2.40 14.81 ------------------------------------------------------------------------------------ 6340233- 821 2394 400747.09 25.04 82.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 239 805786.04 59.02 98.74 1.39- 1.12 239 830115.40 44.43 90.79 1.09- 0.96 239 393174.44 26.85 84.10 0.96- 0.85 239 398501.32 23.81 83.68 0.85- 0.81 239 483058.63 26.26 90.79 0.81- 0.73 239 259369.86 16.02 69.87 0.73- 0.70 239 195050.31 13.38 74.90 0.70- 0.65 239 321878.21 18.34 90.79 0.65- 0.62 239 165519.19 11.42 71.13 0.62- 0.58 243 159062.43 11.13 70.37 ------------------------------------------------------------------------------------ 4.82- 0.58 2394 400747.09 25.04 82.50 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 239 805786.04 59.02 98.74 4.82- 1.12 478 817950.72 51.72 94.77 4.82- 0.96 717 676358.63 43.43 91.21 4.82- 0.85 956 606894.30 38.53 89.33 4.82- 0.81 1195 582127.17 36.07 89.62 4.82- 0.73 1434 528334.28 32.73 86.33 4.82- 0.70 1673 480722.29 29.97 84.70 4.82- 0.65 1912 460866.78 28.51 85.46 4.82- 0.62 2151 428050.38 26.61 83.87 4.82- 0.58 2394 400747.09 25.04 82.50 ------------------------------------------------------------------------------------ 4.82- 0.58 2394 400747.09 25.04 82.50 Scale applied to data: s=0.157723 (maximum obs:6340233.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.031; Rsigma 0.026: data 2394 -> merged 110 With outlier rejection... Rint 0.027; Rsigma 0.026: data 2383 -> merged 110 Rejected total: 11, method kkm 11, method Blessing 0 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585973, 4.832059 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 13.10 100.00 131 1.61 - 1.21 10 10 21.50 100.00 215 1.17 - 1.01 10 10 27.90 100.00 279 0.99 - 0.89 10 10 27.60 100.00 276 0.88 - 0.81 10 10 27.00 100.00 270 0.81 - 0.74 10 10 23.00 100.00 230 0.73 - 0.71 10 10 25.90 100.00 259 0.70 - 0.66 10 10 21.70 100.00 217 0.66 - 0.64 10 10 19.40 100.00 194 0.63 - 0.60 10 10 19.40 100.00 194 --------------------------------------------------------------- 5.92 - 0.60 100 100 22.65 100.00 2265 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:01:14 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919749 5.918019 5.915550 60.0420 90.0632 60.0026 2217 Reflections read from file xs1714a.hkl; mean (I/sigma) = 28.85 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1093 1188 1089 1122 1685 1490 1478 2217 N (int>3sigma) = 0 970 1188 966 1026 1562 1343 1308 1981 Mean intensity = 0.0 53.5 26.5 53.3 58.3 43.9 63.8 61.7 61.4 Mean int/sigma = 0.0 28.3 24.9 27.8 28.2 26.9 29.5 28.9 28.9 Lattice type: P chosen Volume: 146.56 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.918 119.96 90.04 119.96 Niggli form: a.a = 34.989 b.b = 34.994 c.c = 35.023 b.c = -17.482 a.c = -0.026 a.b = -17.473 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.059 CUBIC F-lattice R(int) = 0.195 [ 2064] Vol = 586.2 Cell: 8.364 8.373 8.370 90.01 89.97 90.04 Volume: 586.24 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.052 RHOMBOHEDRAL R-lattice R(int) = 0.182 [ 1789] Vol = 439.7 Cell: 5.916 5.915 14.503 89.98 90.05 119.96 Volume: 439.68 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.052 RHOMBOHEDRAL R-lattice R(int) = 0.161 [ 559] Vol = 439.7 Trigonal Cell: 5.916 5.915 14.503 89.98 90.05 119.96 Volume: 439.68 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.081 TETRAGONAL I-lattice R(int) = 0.158 [ 1821] Vol = 293.1 Cell: 5.919 5.921 8.364 89.95 90.01 90.02 Volume: 293.12 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.057 TETRAGONAL I-lattice R(int) = 0.158 [ 1821] Vol = 293.1 Cell: 5.919 5.921 8.364 89.95 90.01 90.02 Volume: 293.12 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.040 ORTHORHOMBIC I-lattice R(int) = 0.161 [ 1770] Vol = 293.1 Cell: 5.919 8.364 5.921 89.95 89.98 89.99 Volume: 293.12 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.154 [ 1446] Vol = 293.1 Cell: 8.364 5.919 5.921 90.02 90.05 89.99 Volume: 293.12 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.033 MONOCLINIC I-lattice R(int) = 0.150 [ 1459] Vol = 293.1 Cell: 5.918 5.915 8.373 89.98 90.04 89.96 Volume: 293.12 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.051 MONOCLINIC C-lattice R(int) = 0.134 [ 1472] Vol = 293.1 Cell: 8.364 8.373 5.915 89.98 134.96 90.04 Volume: 293.12 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.117 [ 941] Vol = 146.6 Cell: 5.915 5.916 5.918 119.96 90.04 119.96 Volume: 146.56 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1188 0 1479 1490 2217 N (int>3sigma) = 0 0 0 0 1188 0 1323 1343 1981 Mean intensity = 0.0 0.0 0.0 0.0 26.5 0.0 62.9 63.8 61.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.9 0.0 29.5 29.5 28.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.172 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 21 21 162 514 N I>3s 18 18 106 514 0.7 0.7 0.6 31.6 5.8 5.8 3.7 31.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.195 1921 Fd-3m 1 1 227 C N N N N 37 2284 0.196 1959 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364204 8.373435 8.370369 90.0138 89.9718 90.0407 ZERR 1.00 0.000301 0.001719 0.003819 0.0022 0.0127 0.0017 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4875327- 604276 536 529 27 19.6 1345307.09 58.91 0.024 0.026 581458- 137770 699 698 27 25.9 241907.60 27.40 0.032 0.039 118948- 41348 601 601 27 22.3 88185.44 11.45 0.044 0.057 11637- 2009 558 555 29 19.1 3953.18 2.91 0.151 0.197 ------------------------------------------------------------------------------------------- 4875327- 2009 2394 2383 110 21.7 392661.53 24.67 0.027 0.030 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 586 576 27 21.3 697803.09 46.14 0.023 0.024 0.015 1.01-0.78 735 734 28 26.2 377535.93 22.21 0.022 0.027 0.026 0.76-0.65 645 645 28 23.0 277028.52 16.42 0.032 0.038 0.039 0.65-0.59 428 428 27 15.9 182203.43 12.40 0.049 0.052 0.054 ------------------------------------------------------------------------------------------------------ inf-0.59 2394 2383 110 21.7 392661.53 24.67 0.027 0.030 0.026 inf-0.60 2274 2263 99 22.9 406897.45 25.44 0.026 0.029 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 576 27 27 100.0 21.3 697803.09 223.34 0.023 0.004 1.01-0.78 734 28 28 100.0 26.2 377535.93 118.49 0.022 0.005 0.76-0.65 645 28 28 100.0 23.0 277028.52 83.71 0.032 0.009 0.65-0.59 428 27 27 100.0 15.9 182203.43 57.53 0.049 0.017 -------------------------------------------------------------------------------------------- inf-0.59 2383 110 110 100.0 21.7 392661.53 123.47 0.027 0.006 inf-0.60 2263 99 99 100.0 22.9 406897.45 127.77 0.026 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:03:55 2018) ID: 2932; threads 38; handles 878; mem 518736.00 (1229508.00)kB; time: 1w 5d 0h 9m 25s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1200.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 697.1, WS: 297.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1202.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.4,peak PF: 697.1, WS: 299.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:03:55 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000011 0.000010 ) 5.91502 ( 0.00080 ) 5.91640 ( 0.00080 ) 5.92265 ( 0.00063 ) 60.05206 ( 0.01259 ) 89.98756 ( 0.00973 ) 60.01743 ( 0.01418 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:03:55 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021548 -0.014372 0.007204 ( 0.000003 0.000003 0.000002 ) -0.014372 0.028723 -0.014365 ( 0.000003 0.000004 0.000002 ) 0.007204 -0.014365 0.021561 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(13) 89.988(10) 60.017(14) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb PROFFITPEAK info: 1441 peaks in the peak location table UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) 669 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 484 peaks identified as outliers and rejected 474 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 474 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 474 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.032 ( 0.144) | 1.122 ( 0.424) | 1.109 ( 0.575) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.275 ( 0.643) | 1.092 ( 0.634) | 1.12- 0.98 | 47 | 1.019 ( 0.102) | 1.057 ( 0.160) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.029 ( 0.093) | 1.035 ( 0.135) | 1.097 ( 0.433) | 0.89- 0.82 | 47 | 1.036 ( 0.085) | 1.007 ( 0.124) | 1.151 ( 0.478) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.196 ( 0.514) | 0.75- 0.71 | 47 | 1.027 ( 0.045) | 0.938 ( 0.113) | 1.296 ( 0.513) | 0.71- 0.67 | 47 | 1.001 ( 0.040) | 0.889 ( 0.071) | 1.260 ( 0.499) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.301 ( 0.513) | 0.63- 0.59 | 51 | 0.945 ( 0.054) | 0.815 ( 0.041) | 1.344 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 474 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.182 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088653 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010206 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116127 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.018 ( 0.108) | 1.035 ( 0.128) | 0.945 ( 0.327) | 0.97- 0.88 | 47 | 1.028 ( 0.090) | 1.028 ( 0.136) | 1.104 ( 0.406) | 0.88- 0.82 | 47 | 1.044 ( 0.079) | 1.018 ( 0.119) | 1.200 ( 0.515) | 0.82- 0.75 | 47 | 1.039 ( 0.079) | 0.988 ( 0.125) | 1.098 ( 0.421) | 0.75- 0.71 | 47 | 1.020 ( 0.045) | 0.932 ( 0.110) | 1.313 ( 0.542) | 0.71- 0.67 | 47 | 0.997 ( 0.044) | 0.883 ( 0.075) | 1.208 ( 0.469) | 0.67- 0.63 | 47 | 0.975 ( 0.046) | 0.843 ( 0.040) | 1.300 ( 0.488) | 0.63- 0.59 | 48 | 0.949 ( 0.045) | 0.811 ( 0.041) | 1.349 ( 0.524) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.015 ( 0.090) | 0.993 ( 0.294) | 1.174 ( 0.534) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.3 | 180 | 1.118 ( 0.115) | 1.243 ( 0.460) | 1.179 ( 0.612) | 13.3-19.0 | 180 | 1.083 ( 0.056) | 1.135 ( 0.282) | 1.206 ( 0.518) | 19.0-23.2 | 180 | 1.071 ( 0.072) | 1.147 ( 0.387) | 1.165 ( 0.499) | 23.2-27.2 | 180 | 1.037 ( 0.079) | 1.072 ( 0.283) | 1.197 ( 0.574) | 27.2-30.8 | 180 | 1.014 ( 0.076) | 1.016 ( 0.260) | 1.195 ( 0.511) | 30.8-33.8 | 180 | 0.985 ( 0.084) | 0.925 ( 0.098) | 1.192 ( 0.514) | 33.8-37.0 | 180 | 0.967 ( 0.078) | 0.902 ( 0.097) | 1.185 ( 0.485) | 37.0-39.7 | 180 | 0.951 ( 0.091) | 0.874 ( 0.141) | 1.184 ( 0.553) | 39.7-42.7 | 180 | 0.928 ( 0.081) | 0.836 ( 0.080) | 1.187 ( 0.517) | 42.8-49.9 | 178 | 0.941 ( 0.082) | 0.816 ( 0.065) | 1.156 ( 0.452) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1798 | 1.010 ( 0.104) | 0.997 ( 0.289) | 1.185 ( 0.526) | Fitted profile normalization line parameters e1 dimension: a=-0.0046 b=1.16 e2 dimension: a=-0.0097 b=1.26 e3 dimension: a=0.0019 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:04:14 2018 PROFFITMAIN - Started at Tue Mar 27 15:04:14 2018 OTKP changes: 1798 2 3 4 OTKP changes: 1798 2 3 4 UB - matrix: -0.070171 0.031113 0.088940 ( 0.000012 0.000012 0.000011 ) -0.068699 -0.065917 -0.010407 ( 0.000012 0.000013 0.000012 ) 0.109150 -0.153013 0.116315 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021557 -0.014356 0.007170 ( 0.000003 0.000002 0.000002 ) -0.014356 0.028726 -0.014344 ( 0.000002 0.000004 0.000002 ) 0.007170 -0.014344 0.021548 ( 0.000002 0.000002 0.000003 ) UB fit with 1798 obs out of 1798 (total:1798,skipped:0) (100.00%) unit cell: 5.9144(7) 5.9136(7) 5.9139(6) 60.043(12) 90.003(9) 60.013(13) V = 146.38(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070040 0.030657 0.088975 ( 0.000029 0.000028 0.000016 ) -0.068253 -0.066143 -0.010488 ( 0.000026 0.000025 0.000015 ) 0.109063 -0.153049 0.115957 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021459 -0.014325 0.007131 ( 0.000008 0.000006 0.000004 ) -0.014325 0.028739 -0.014326 ( 0.000006 0.000008 0.000005 ) 0.007131 -0.014326 0.021472 ( 0.000004 0.000005 0.000004 ) unit cell: 5.9276(14) 5.9136(14) 5.9249(11) 60.01(2) 89.960(18) 60.00(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070330 0.030934 0.088801 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066129 -0.010682 ( 0.000024 0.000023 0.000013 ) 0.109331 -0.153280 0.116361 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014410 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014410 0.028825 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014382 0.021540 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9161(13) 5.9077(13) 5.9184(10) 60.05(2) 90.068(16) 60.00(2) V = 146.28(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.796) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070330 0.030934 0.088801 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066129 -0.010682 ( 0.000024 0.000023 0.000013 ) 0.109331 -0.153280 0.116361 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014410 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014410 0.028825 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014382 0.021540 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9161(13) 5.9077(13) 5.9184(10) 60.05(2) 90.068(16) 60.00(2) V = 146.28(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070330 0.030934 0.088801 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066129 -0.010682 ( 0.000024 0.000023 0.000013 ) 0.109331 -0.153280 0.116361 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021579 -0.014410 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014410 0.028825 -0.014382 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014382 0.021540 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9161(13) 5.9077(13) 5.9184(10) 60.05(2) 90.068(16) 60.00(2) V = 146.28(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070409 0.031360 0.088642 ( 0.000026 0.000023 0.000028 ) -0.068573 -0.066013 -0.010220 ( 0.000031 0.000027 0.000033 ) 0.108984 -0.152622 0.116241 ( 0.000020 0.000017 0.000022 ) M - matrix: 0.021537 -0.014315 0.007128 ( 0.000007 0.000005 0.000005 ) -0.014315 0.028635 -0.014286 ( 0.000005 0.000007 0.000005 ) 0.007128 -0.014286 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(17) 5.9211(17) 5.9219(14) 60.03(3) 89.94(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070359 0.031207 0.088838 ( 0.000023 0.000020 0.000025 ) -0.068784 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109161 -0.153142 0.116575 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014383 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014383 0.028763 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014398 0.021589 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9097(16) 5.9166(16) 5.9146(12) 59.94(2) 89.949(19) 60.01(3) V = 146.19(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.796) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070359 0.031207 0.088838 ( 0.000023 0.000020 0.000025 ) -0.068784 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109161 -0.153142 0.116575 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014383 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014383 0.028763 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014398 0.021589 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9097(16) 5.9166(16) 5.9146(12) 59.94(2) 89.949(19) 60.01(3) V = 146.19(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070359 0.031207 0.088838 ( 0.000023 0.000020 0.000025 ) -0.068784 -0.065854 -0.010354 ( 0.000030 0.000026 0.000032 ) 0.109161 -0.153142 0.116575 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021598 -0.014383 0.007187 ( 0.000007 0.000005 0.000005 ) -0.014383 0.028763 -0.014398 ( 0.000005 0.000006 0.000005 ) 0.007187 -0.014398 0.021589 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9097(16) 5.9166(16) 5.9146(12) 59.94(2) 89.949(19) 60.01(3) V = 146.19(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.070172 0.031456 0.088647 ( 0.000017 0.000026 0.000022 ) -0.068861 -0.065702 -0.010200 ( 0.000021 0.000032 0.000027 ) 0.108910 -0.152876 0.116138 ( 0.000016 0.000026 0.000021 ) M - matrix: 0.021527 -0.014333 0.007130 ( 0.000005 0.000005 0.000004 ) -0.014333 0.028677 -0.014296 ( 0.000005 0.000009 0.000005 ) 0.007130 -0.014296 0.021450 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9183(15) 5.9194(15) 5.9266(11) 60.02(2) 89.941(18) 59.99(3) V = 146.91(5) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 UB - matrix: -0.070126 0.031443 0.088891 ( 0.000016 0.000025 0.000021 ) -0.068729 -0.066005 -0.009957 ( 0.000018 0.000028 0.000024 ) 0.109180 -0.153115 0.116562 ( 0.000016 0.000024 0.000021 ) M - matrix: 0.021562 -0.014386 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014386 0.028790 -0.014395 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014395 0.021588 ( 0.000004 0.000005 0.000006 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 5.9163(14) 5.9140(14) 5.9129(11) 59.97(2) 89.936(17) 59.97(2) V = 146.24(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.796) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070126 0.031443 0.088891 ( 0.000016 0.000025 0.000021 ) -0.068729 -0.066005 -0.009957 ( 0.000018 0.000028 0.000024 ) 0.109180 -0.153115 0.116562 ( 0.000016 0.000024 0.000021 ) M - matrix: 0.021562 -0.014386 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014386 0.028790 -0.014395 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014395 0.021588 ( 0.000004 0.000005 0.000006 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 5.9163(14) 5.9140(14) 5.9129(11) 59.97(2) 89.936(17) 59.97(2) V = 146.24(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070126 0.031443 0.088891 ( 0.000016 0.000025 0.000021 ) -0.068729 -0.066005 -0.009957 ( 0.000018 0.000028 0.000024 ) 0.109180 -0.153115 0.116562 ( 0.000016 0.000024 0.000021 ) M - matrix: 0.021562 -0.014386 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014386 0.028790 -0.014395 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014395 0.021588 ( 0.000004 0.000005 0.000006 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 5.9163(14) 5.9140(14) 5.9129(11) 59.97(2) 89.936(17) 59.97(2) V = 146.24(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070051 0.031091 0.088897 ( 0.000012 0.000013 0.000012 ) -0.068682 -0.065802 -0.010459 ( 0.000014 0.000015 0.000014 ) 0.109197 -0.153060 0.116404 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021548 -0.014372 0.007202 ( 0.000003 0.000003 0.000002 ) -0.014372 0.028724 -0.014365 ( 0.000003 0.000004 0.000002 ) 0.007202 -0.014365 0.021562 ( 0.000002 0.000002 0.000003 ) UB fit with 1798 obs out of 1798 (total:1798,skipped:0) (100.00%) unit cell: 5.9197(8) 5.9179(8) 5.9153(6) 60.042(13) 90.058(10) 60.000(14) V = 146.55(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 59 reflections under beam stop or inside a detector rejection region 17 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof 2445 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:04:18 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.796) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.796) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.796) PROFFIT INFO: signal sum: min=249.0000 max=20928218.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2972886.5433 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4756618.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47803.1875 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=248.73 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 14 91 225 493 551 958 1604 2228 2445 Percent 0.0 0.0 0.6 3.7 9.2 20.2 22.5 39.2 65.6 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2445 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2445 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4756619- 1230286 244 1986324.94 121.44 100.00 1228602- 712302 244 934153.93 107.13 100.00 711801- 286326 244 465485.23 98.06 100.00 285930- 181394 244 220246.42 75.61 100.00 181167- 136464 244 159845.82 52.47 100.00 136438- 103330 244 116736.06 37.60 100.00 103180- 79454 244 91102.48 30.33 100.00 79404- 5943 244 45861.92 20.77 100.00 5927- 3241 244 4288.10 5.56 97.95 3234- 924 249 2473.56 4.04 65.46 ------------------------------------------------------------------------------------ 4756619- 924 2445 401833.49 55.20 96.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 244 747618.08 89.60 99.18 1.28- 1.05 244 572823.88 67.91 97.54 1.05- 0.92 244 494553.56 62.47 97.95 0.92- 0.82 244 359922.62 53.44 96.31 0.82- 0.74 244 436822.75 58.42 97.13 0.74- 0.67 244 400471.90 57.69 96.72 0.67- 0.61 244 239233.51 41.79 95.90 0.61- 0.56 244 329091.29 48.38 93.85 0.56- 0.51 244 238167.41 39.26 93.44 0.51- 0.40 249 203690.16 33.43 94.78 ------------------------------------------------------------------------------------ 5.26- 0.40 2445 401833.49 55.20 96.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:04:19 2018 Sorting 2445 observations 283 unique observations with > 7.00 F2/sig(F2) 2445 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 Total number of frames 421 Maximum number of 283 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2445 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 Total number of frames 213 1973 observations > 7.00 F2/sig(F2) 1973 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 Total number of frames 213 Removing 'redundancy=1' reflections Average redundancy: 7.3 (Out of 1973 removed 36 = 1937, unique = 265) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 1937 observations in 4 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 Total number of frames 213 265 unique data precomputed (should be 265) 265 unique data with 1937 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.3 (Out of 1937 removed 0 = 1937, unique = 265) 265 unique data precomputed (should be 265) 265 unique data with 1937 observations RMS deviation of equivalent data = 0.71275 Rint = 0.68274 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66019, wR= 3.53721 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68189, wR= 2.80267, Acormin=0.043, Acormax=1.897, Acor_av=0.766 F test: Probability=0.000, F= 0.935 Trying model 2 (ne=2, no=1)... Results: Rint= 0.84478, wR= 2.60831, Acormin=-0.526, Acormax=1.656, Acor_av=0.444 F test: Probability=0.000, F= 0.608 Trying model 3 (ne=4, no=0)... Results: Rint= 0.72258, wR= 2.41848, Acormin=-0.065, Acormax=2.198, Acor_av=0.634 F test: Probability=0.000, F= 0.828 Trying model 4 (ne=4, no=1)... Results: Rint= 0.89107, wR= 2.26074, Acormin=-0.412, Acormax=1.826, Acor_av=0.344 F test: Probability=0.000, F= 0.543 Trying model 5 (ne=4, no=3)... Results: Rint= 0.93959, wR= 2.06807, Acormin=-1.033, Acormax=1.748, Acor_av=0.201 F test: Probability=0.000, F= 0.487 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75741, wR= 2.42705, Acormin=-0.311, Acormax=2.505, Acor_av=0.539 F test: Probability=0.000, F= 0.747 Trying model 7 (ne=6, no=1)... Results: Rint= 0.91121, wR= 2.32400, Acormin=-0.565, Acormax=1.922, Acor_av=0.273 F test: Probability=0.000, F= 0.515 Trying model 8 (ne=6, no=3)... Results: Rint= 0.94819, wR= 2.14081, Acormin=-1.621, Acormax=1.955, Acor_av=0.149 F test: Probability=0.000, F= 0.474 Trying model 9 (ne=6, no=5)... Results: Rint= 0.93472, wR= 2.14701, Acormin=-1.245, Acormax=1.785, Acor_av=0.133 F test: Probability=0.000, F= 0.484 Trying model 10 (ne=8, no=0)... Results: Rint= 0.85239, wR= 2.25909, Acormin=-0.623, Acormax=2.516, Acor_av=0.383 F test: Probability=0.000, F= 0.584 Trying model 11 (ne=8, no=1)... Results: Rint= 0.99457, wR= 1.82971, Acormin=-1.352, Acormax=1.488, Acor_av=0.107 F test: Probability=0.000, F= 0.428 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98848, wR= 1.46144, Acormin=-0.043, Acormax=0.070, Acor_av=0.001 F test: Probability=0.000, F= 0.432 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99824, wR= 1.50743, Acormin=-0.042, Acormax=0.092, Acor_av=0.002 F test: Probability=0.000, F= 0.420 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00723, wR= 1.65723, Acormin=-0.041, Acormax=0.085, Acor_av=0.002 F test: Probability=0.000, F= 0.409 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.85001 There are 213 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 217 pars with 23653 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71275 Using Levenberg-Marquardt: 0.00010 New wR= 0.69110 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68274 with corrections 0.65585 Rint for all data: 0.85001 with corrections 0.83064 14 observations identified as outliers and rejected Cycle 2 wR= 0.65811 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 New wR= 0.69081 Using Levenberg-Marquardt: 0.01000 New wR= 0.65523 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65737 with corrections 0.63399 Rint for all data: 0.85001 with corrections 0.83477 11 observations identified as outliers and rejected Cycle 3 wR= 0.63676 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63551 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64723 with corrections 0.62842 Rint for all data: 0.85001 with corrections 0.83778 9 observations identified as outliers and rejected Cycle 4 wR= 0.61732 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61476 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64315 with corrections 0.62967 Rint for all data: 0.85001 with corrections 0.83958 8 observations identified as outliers and rejected Cycle 5 wR= 0.59422 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.59010 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64141 with corrections 0.62690 Rint for all data: 0.85001 with corrections 0.83860 2 observations identified as outliers and rejected Final wR= 0.59010 Final frame scales: Min= 0.6324 Max= 4.7207 Final absorption correction factors: Amin= 0.3713 Amax= 1.3860 PROFFIT INFO: Inet (after scale3 abspack): min=762.4305 max=6408645.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=132.5834 max=74767.9609 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/4 frame:1/109 2445 reflections read from tmp file 1885 reflections are rejected (1803 as outliers, 82 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8+ Number of groups: 0 82 40 25 13 11 3 3 Initial Chi^2= 0.55035 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.83752 Current error model SIG(F2)^2 = 210.38*I_RAW + 0.00*I_BACK+(0.01910*)^2 Cycle 2, Chi^2= 1.00196 Current error model SIG(F2)^2 = 153.65*I_RAW + 0.00*I_BACK+(0.02407*)^2 Cycle 3, Chi^2= 1.00652 Current error model SIG(F2)^2 = 167.63*I_RAW + 0.00*I_BACK+(0.01948*)^2 Cycle 4, Chi^2= 0.99881 Current error model SIG(F2)^2 = 159.69*I_RAW + 0.00*I_BACK+(0.02233*)^2 Cycle 5, Chi^2= 1.00213 Current error model SIG(F2)^2 = 165.30*I_RAW + 0.00*I_BACK+(0.02042*)^2 Cycle 6, Chi^2= 0.99917 Current error model SIG(F2)^2 = 161.79*I_RAW + 0.00*I_BACK+(0.02166*)^2 Cycle 7, Chi^2= 1.00080 Current error model SIG(F2)^2 = 164.18*I_RAW + 0.00*I_BACK+(0.02084*)^2 Cycle 8, Chi^2= 0.99958 Current error model SIG(F2)^2 = 162.64*I_RAW + 0.00*I_BACK+(0.02137*)^2 Cycle 9, Chi^2= 1.00032 Current error model SIG(F2)^2 = 163.67*I_RAW + 0.00*I_BACK+(0.02102*)^2 Cycle 10, Chi^2= 0.99981 Current error model SIG(F2)^2 = 163.00*I_RAW + 0.00*I_BACK+(0.02125*)^2 Final Chi^2= 0.99981 Final error model SIG(F2)^2 = 163.00*I_RAW + 0.00*I_BACK+(0.02125*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6408645- 1225274 244 1992084.33 102.96 100.00 1218076- 660744 244 897382.80 55.87 100.00 659144- 267888 244 431251.38 48.56 100.00 267535- 177048 244 216401.57 35.89 100.00 176877- 136229 244 153925.11 25.16 100.00 136139- 99247 244 118650.27 20.30 100.00 99214- 70109 244 84748.03 15.49 100.00 70053- 6256 244 40547.62 11.43 95.90 6221- 3007 244 4216.50 3.83 79.10 3000- 762 249 2256.43 3.02 46.99 ------------------------------------------------------------------------------------ 6408645- 762 2445 393344.99 32.19 92.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 244 825488.78 67.02 97.13 1.28- 1.05 244 581243.47 47.42 95.90 1.05- 0.92 244 511607.85 37.83 94.26 0.92- 0.82 244 360172.60 30.59 89.75 0.82- 0.74 244 436581.11 29.86 94.26 0.74- 0.67 244 372591.72 29.17 91.80 0.67- 0.61 244 218231.99 21.39 88.52 0.61- 0.56 244 287633.13 22.93 90.16 0.56- 0.51 244 195253.66 19.69 88.52 0.51- 0.40 249 149639.58 16.36 90.76 ------------------------------------------------------------------------------------ 5.26- 0.40 2445 393344.99 32.19 92.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 244 825488.78 67.02 97.13 5.26- 1.05 488 703366.12 57.22 96.52 5.26- 0.92 732 639446.70 50.75 95.77 5.26- 0.82 976 569628.18 45.71 94.26 5.26- 0.74 1220 543018.76 42.54 94.26 5.26- 0.67 1464 514614.25 40.31 93.85 5.26- 0.61 1708 472273.93 37.61 93.09 5.26- 0.56 1952 449193.83 35.77 92.73 5.26- 0.51 2196 420978.26 33.99 92.26 5.26- 0.40 2445 393344.99 32.19 92.11 ------------------------------------------------------------------------------------ 5.26- 0.40 2445 393344.99 32.19 92.11 Scale applied to data: s=0.156039 (maximum obs:6408645.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.839; Rsigma 0.021: data 2445 -> merged 313 With outlier rejection... Rint 0.761; Rsigma 0.021: data 2273 -> merged 313 Rejected total: 172, method kkm 159, method Blessing 13 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404362, 5.272232 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 10.73 100.00 161 1.46 - 1.12 15 15 17.33 100.00 260 1.08 - 0.96 15 15 15.07 100.00 226 0.96 - 0.86 15 15 13.67 100.00 205 0.86 - 0.79 15 15 12.07 100.00 181 0.79 - 0.73 15 15 10.60 100.00 159 0.73 - 0.69 15 15 9.60 100.00 144 0.69 - 0.65 15 15 9.60 100.00 144 0.65 - 0.63 15 15 5.80 100.00 87 0.63 - 0.60 21 21 6.24 100.00 131 --------------------------------------------------------------- 5.92 - 0.60 156 156 10.88 100.00 1698 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:04:19 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919675 5.917922 5.915311 60.0418 90.0579 59.9999 2272 Reflections read from file xs1714a.hkl; mean (I/sigma) = 31.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1116 1211 1117 1152 1722 1519 1511 2272 N (int>3sigma) = 0 1023 1211 1024 1099 1629 1413 1386 2096 Mean intensity = 0.0 51.3 25.2 50.9 55.8 42.0 60.1 58.3 58.2 Mean int/sigma = 0.0 31.0 27.2 30.5 31.1 29.5 32.0 31.5 31.5 Lattice type: P chosen Volume: 146.55 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.918 119.96 90.04 119.96 Niggli form: a.a = 34.990 b.b = 34.991 c.c = 35.022 b.c = -17.481 a.c = -0.025 a.b = -17.474 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.202 [ 2119] Vol = 586.2 Cell: 8.364 8.373 8.370 90.02 89.97 90.04 Volume: 586.20 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.049 RHOMBOHEDRAL R-lattice R(int) = 0.185 [ 1844] Vol = 439.6 Cell: 5.915 5.915 14.503 89.98 90.04 119.96 Volume: 439.65 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.049 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 586] Vol = 439.6 Trigonal Cell: 5.915 5.915 14.503 89.98 90.04 119.96 Volume: 439.65 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.080 TETRAGONAL I-lattice R(int) = 0.163 [ 1875] Vol = 293.1 Cell: 5.919 5.920 8.364 89.95 90.01 90.02 Volume: 293.10 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.054 TETRAGONAL I-lattice R(int) = 0.163 [ 1875] Vol = 293.1 Cell: 5.919 5.920 8.364 89.95 90.01 90.02 Volume: 293.10 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.037 ORTHORHOMBIC I-lattice R(int) = 0.169 [ 1825] Vol = 293.1 Cell: 5.919 8.364 5.920 89.95 89.98 89.99 Volume: 293.10 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.159 [ 1500] Vol = 293.1 Cell: 8.364 5.919 5.920 90.02 90.05 89.99 Volume: 293.10 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.032 MONOCLINIC I-lattice R(int) = 0.153 [ 1512] Vol = 293.1 Cell: 5.918 5.915 8.373 89.98 90.04 89.96 Volume: 293.10 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.053 MONOCLINIC C-lattice R(int) = 0.140 [ 1525] Vol = 293.1 Cell: 8.364 8.373 5.915 89.98 134.97 90.04 Volume: 293.10 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.120 [ 994] Vol = 146.5 Cell: 5.915 5.915 5.918 119.96 90.04 119.96 Volume: 146.55 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1211 0 1516 1519 2272 N (int>3sigma) = 0 0 0 0 1211 0 1392 1413 2096 Mean intensity = 0.0 0.0 0.0 0.0 25.2 0.0 58.8 60.1 58.2 Mean int/sigma = 0.0 0.0 0.0 0.0 27.2 0.0 31.9 32.0 31.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.177 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 23 23 166 530 N I>3s 20 20 125 530 0.7 0.7 0.6 30.0 6.9 6.9 4.1 33.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.202 1972 Fd-3m 1 1 227 C N N N N 37 2284 0.202 2010 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364370 8.372827 8.370252 90.0151 89.9741 90.0423 ZERR 1.00 0.000303 0.001721 0.003815 0.0022 0.0127 0.0016 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3348356- 648713 389 362 31 11.7 1004191.17 55.68 0.657 0.649 648239- 486480 322 314 31 10.1 555410.27 47.00 0.884 0.804 484707- 369304 258 246 31 7.9 406497.12 33.97 0.896 0.844 369042- 300469 305 292 31 9.4 305919.21 28.67 0.907 0.948 291116- 219565 243 212 31 6.8 214085.44 25.90 0.897 0.919 215960- 160693 265 234 31 7.5 145966.15 24.03 0.630 0.713 159449- 94569 259 241 31 7.8 103400.69 18.15 0.529 0.524 92475- 68065 160 146 31 4.7 82352.13 15.64 0.425 0.245 67670- 47315 134 122 31 3.9 58815.44 12.87 0.437 0.284 47141- 1735 110 104 34 3.1 23327.30 6.95 0.717 0.670 ------------------------------------------------------------------------------------------- 3348356- 1735 2445 2273 313 7.3 375419.89 31.55 0.761 0.739 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 473 444 31 14.3 679685.94 56.44 0.749 0.797 0.014 1.05-0.83 452 435 32 13.6 440025.09 34.71 0.875 1.018 0.019 0.82-0.72 367 356 32 11.1 385430.50 28.38 0.742 0.785 0.025 0.72-0.65 302 283 32 8.8 266657.69 24.96 0.804 0.804 0.026 0.64-0.60 229 201 31 6.5 248755.72 21.66 0.767 0.754 0.029 0.59-0.56 180 165 33 5.0 184806.50 18.30 0.586 0.546 0.034 0.56-0.52 160 143 31 4.6 221915.17 21.33 0.622 0.668 0.032 0.52-0.49 126 108 31 3.5 136521.33 15.62 0.651 0.475 0.038 0.49-0.46 93 81 31 2.6 165948.56 17.62 0.386 0.268 0.037 0.45-0.40 63 57 29 2.0 123641.88 14.71 0.240 0.187 0.043 ------------------------------------------------------------------------------------------------------ inf-0.40 2445 2273 313 7.3 375419.89 31.55 0.761 0.739 0.021 inf-0.60 1801 1699 156 10.9 442785.82 36.05 0.787 0.839 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 444 31 31 100.0 14.3 679685.94 250.36 0.749 0.005 1.05-0.83 435 32 32 100.0 13.6 440025.09 157.10 0.875 0.007 0.82-0.72 356 32 32 100.0 11.1 385430.50 117.01 0.742 0.010 0.72-0.65 283 32 32 100.0 8.8 266657.69 95.58 0.804 0.013 0.64-0.60 201 31 31 100.0 6.5 248755.72 73.02 0.767 0.015 0.59-0.56 165 36 33 91.7 5.0 184806.50 53.09 0.586 0.018 0.56-0.52 143 34 31 91.2 4.6 221915.17 58.26 0.622 0.017 0.52-0.49 108 45 31 68.9 3.5 136521.33 37.65 0.651 0.025 0.49-0.46 81 61 31 50.8 2.6 165948.56 34.85 0.386 0.026 0.45-0.40 57 127 29 22.8 2.0 123641.88 22.65 0.240 0.030 -------------------------------------------------------------------------------------------- inf-0.40 2273 462 313 67.7 7.3 375419.89 126.77 0.761 0.012 inf-0.60 1699 156 156 100.0 10.9 442785.82 153.90 0.787 0.008 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: -0.024968 -0.079473 -0.015545 ( 0.000007 0.000007 0.000006 ) 0.072472 -0.029111 0.032901 ( 0.000007 0.000008 0.000007 ) -0.036270 -0.003604 0.076530 ( 0.000005 0.000006 0.000005 ) M - matrix: 0.007191 0.000005 -0.000003 ( 0.000001 0.000001 0.000001 ) 0.000005 0.007176 0.000002 ( 0.000001 0.000001 0.000001 ) -0.000003 0.000002 0.007181 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024968 -0.079473 -0.015545 ( 0.000007 0.000007 0.000006 ) 0.072472 -0.029111 0.032901 ( 0.000007 0.000008 0.000007 ) -0.036270 -0.003604 0.076530 ( 0.000005 0.000006 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3644(7) 8.3729(7) 8.3703(6) 90.015(6) 89.974(6) 90.042(7) V = 586.21(8) unit cell: 8.3692(2) 8.3692(2) 8.3692(2) 90.0 90.0 90.0 V = 586.21(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.796) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.796) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.796) PROFFIT INFO: signal sum: min=249.0000 max=20928218.0000 PROFFIT INFO: signal sum lp corr: min=577.4800 max=2972886.5433 PROFFIT INFO: background sum: min=729.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=923.9680 max=4756618.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47803.1875 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=248.73 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 28 182 450 986 1102 1916 3208 4456 4890 Percent 0.0 0.0 0.6 3.7 9.2 20.2 22.5 39.2 65.6 91.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2445 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2445 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4756619- 1230286 244 1986324.94 121.44 100.00 1228602- 712302 244 934153.93 107.13 100.00 711801- 286326 244 465485.23 98.06 100.00 285930- 181394 244 220246.42 75.61 100.00 181167- 136464 244 159845.82 52.47 100.00 136438- 103330 244 116736.06 37.60 100.00 103180- 79454 244 91102.48 30.33 100.00 79404- 5943 244 45861.92 20.77 100.00 5927- 3241 244 4288.10 5.56 97.95 3234- 924 249 2473.56 4.04 65.46 ------------------------------------------------------------------------------------ 4756619- 924 2445 401833.49 55.20 96.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 244 776805.25 96.24 100.00 1.39- 1.12 244 795130.10 64.86 100.00 1.12- 0.96 244 421057.11 69.64 97.54 0.96- 0.88 244 392684.43 63.06 96.72 0.88- 0.81 244 494590.27 71.69 99.59 0.81- 0.73 244 265978.83 42.88 99.59 0.73- 0.71 244 184108.37 33.98 86.07 0.70- 0.65 244 351107.38 51.00 96.31 0.65- 0.62 244 173858.62 29.81 90.16 0.62- 0.58 249 167810.04 29.33 96.79 ------------------------------------------------------------------------------------ 4.82- 0.58 2445 401833.49 55.20 96.28 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:04:20 2018 Sorting 2445 observations 85 unique observations with > 7.00 F2/sig(F2) 2445 observations in 4 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 Total number of frames 421 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 2445 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 Total number of frames 86 1973 observations > 7.00 F2/sig(F2) 1973 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 Total number of frames 86 Removing 'redundancy=1' reflections Average redundancy: 21.2 (Out of 1973 removed 3 = 1970, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 1970 observations in 4 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 Total number of frames 86 93 unique data precomputed (should be 93) 93 unique data with 1970 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.2 (Out of 1970 removed 0 = 1970, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 1970 observations RMS deviation of equivalent data = 0.13642 Rint = 0.10589 4 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.10496, wR= 0.13512 Trying model 1 (ne=2, no=0)... Results: Rint= 0.07704, wR= 0.09480, Acormin=0.811, Acormax=1.244, Acor_av=0.976 F test: Probability=1.000, F= 1.851 Trying model 2 (ne=2, no=1)... Results: Rint= 0.07046, wR= 0.08771, Acormin=0.744, Acormax=1.299, Acor_av=0.943 F test: Probability=1.000, F= 1.194 Trying model 3 (ne=4, no=0)... Results: Rint= 0.06466, wR= 0.08241, Acormin=0.750, Acormax=1.306, Acor_av=0.947 F test: Probability=1.000, F= 1.184 Trying model 4 (ne=4, no=1)... Results: Rint= 0.06049, wR= 0.07835, Acormin=0.680, Acormax=1.283, Acor_av=0.889 F test: Probability=0.998, F= 1.141 Trying model 5 (ne=4, no=3)... Results: Rint= 0.04803, wR= 0.06566, Acormin=0.648, Acormax=1.318, Acor_av=0.879 F test: Probability=1.000, F= 1.580 Trying model 6 (ne=6, no=0)... Results: Rint= 0.06252, wR= 0.07982, Acormin=0.747, Acormax=1.304, Acor_av=0.943 F test: Probability=0.000, F= 0.589 Trying model 7 (ne=6, no=1)... Results: Rint= 0.05790, wR= 0.07577, Acormin=0.686, Acormax=1.292, Acor_av=0.880 F test: Probability=0.000, F= 0.686 Trying model 8 (ne=6, no=3)... Results: Rint= 0.04649, wR= 0.06313, Acormin=0.638, Acormax=1.329, Acor_av=0.881 F test: Probability=0.894, F= 1.060 Trying model 9 (ne=6, no=5)... Results: Rint= 0.04127, wR= 0.05701, Acormin=0.551, Acormax=1.292, Acor_av=0.839 F test: Probability=1.000, F= 1.337 Trying model 10 (ne=8, no=0)... Results: Rint= 0.05904, wR= 0.07614, Acormin=0.694, Acormax=1.308, Acor_av=0.930 F test: Probability=0.000, F= 0.490 Trying model 11 (ne=8, no=1)... Results: Rint= 0.04926, wR= 0.06458, Acormin=0.680, Acormax=1.418, Acor_av=0.922 F test: Probability=0.000, F= 0.702 Trying model 12 (ne=8, no=3)... Results: Rint= 0.04265, wR= 0.05775, Acormin=0.511, Acormax=1.124, Acor_av=0.731 F test: Probability=0.000, F= 0.933 Trying model 13 (ne=8, no=5)... Results: Rint= 0.03693, wR= 0.05188, Acormin=0.478, Acormax=1.192, Acor_av=0.770 F test: Probability=1.000, F= 1.237 Trying model 14 (ne=8, no=7)... Results: Rint= 0.03443, wR= 0.04829, Acormin=0.489, Acormax=1.246, Acor_av=0.790 F test: Probability=0.997, F= 1.141 Final absorption model (ne=8, no=7): Rint= 0.03443, Acormin=0.489, Acormax=1.246, Acor_av=0.790 Combined refinement in use Rint: 0.10603 There are 86 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 8, max odd order: 7 (80 parameters) Refinement control: 165 pars with 13695 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.13642 Using Levenberg-Marquardt: 0.00010 New wR= 0.04217 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10589 with corrections 0.03049 Rint for all data: 0.10603 with corrections 0.03071 4 observations identified as outliers and rejected Cycle 2 wR= 0.03925 Using Levenberg-Marquardt: 0.00001 New wR= 0.03802 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10547 with corrections 0.02789 Rint for all data: 0.10603 with corrections 0.03079 1 observations identified as outliers and rejected Cycle 3 wR= 0.03723 Using Levenberg-Marquardt: 0.00000 New wR= 0.03703 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10545 with corrections 0.02781 Rint for all data: 0.10603 with corrections 0.03062 0 observations identified as outliers and rejected Cycle 4 wR= 0.03703 Using Levenberg-Marquardt: 0.00000 New wR= 0.03694 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10545 with corrections 0.02778 Rint for all data: 0.10603 with corrections 0.03053 0 observations identified as outliers and rejected Cycle 5 wR= 0.03694 Using Levenberg-Marquardt: 0.00000 New wR= 0.03690 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.10545 with corrections 0.02777 Rint for all data: 0.10603 with corrections 0.03048 0 observations identified as outliers and rejected Final wR= 0.03690 Final frame scales: Min= 0.8579 Max= 1.1099 Final absorption correction factors: Amin= 0.5613 Amax= 1.2916 PROFFIT INFO: Inet (after scale3 abspack): min=834.2195 max=6298767.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=136.5886 max=49361.8125 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/4 frame:1/109 2445 reflections read from tmp file 274 reflections are rejected (272 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 2 0 5 4 4 2 85 Initial Chi^2= 0.34044 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.27784 Current error model SIG(F2)^2 = 160.35*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 365.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 365.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6298767- 1262267 244 2012769.73 80.32 100.00 1241282- 681874 244 910773.31 36.67 100.00 680154- 300217 244 462386.84 37.25 100.00 299741- 177517 244 220913.00 27.05 100.00 177506- 143993 244 160395.42 18.13 100.00 143904- 99053 244 114364.29 13.05 100.00 99013- 78130 244 88785.11 10.68 100.00 77971- 5760 244 46176.00 7.69 87.70 5723- 3188 244 4150.75 2.70 15.57 3179- 834 249 2489.70 2.25 10.84 ------------------------------------------------------------------------------------ 6298767- 834 2445 401502.77 23.54 81.27 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 244 807953.16 55.75 99.18 1.39- 1.12 244 806402.16 41.19 87.30 1.12- 0.96 244 420395.27 25.84 83.20 0.96- 0.88 244 392607.89 22.17 83.61 0.88- 0.81 244 488967.92 24.76 89.75 0.81- 0.73 244 258127.05 15.09 68.03 0.73- 0.71 244 180509.15 12.07 70.49 0.70- 0.65 244 339005.29 17.68 91.39 0.65- 0.62 244 165428.24 10.63 70.08 0.62- 0.58 249 160568.70 10.46 69.88 ------------------------------------------------------------------------------------ 4.82- 0.58 2445 401502.77 23.54 81.27 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 244 807953.16 55.75 99.18 4.82- 1.12 488 807177.66 48.47 93.24 4.82- 0.96 732 678250.20 40.93 89.89 4.82- 0.88 976 606839.62 36.24 88.32 4.82- 0.81 1220 583265.28 33.94 88.61 4.82- 0.73 1464 529075.57 30.80 85.18 4.82- 0.71 1708 479280.37 28.12 83.08 4.82- 0.65 1952 461745.99 26.82 84.12 4.82- 0.62 2196 428821.79 25.02 82.56 4.82- 0.58 2445 401502.77 23.54 81.27 ------------------------------------------------------------------------------------ 4.82- 0.58 2445 401502.77 23.54 81.27 Scale applied to data: s=0.158761 (maximum obs:6298767.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.030; Rsigma 0.027: data 2445 -> merged 110 With outlier rejection... Rint 0.027; Rsigma 0.028: data 2433 -> merged 110 Rejected total: 12, method kkm 10, method Blessing 2 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585960, 4.831953 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 13.20 100.00 132 1.61 - 1.21 10 10 22.20 100.00 222 1.17 - 1.01 10 10 28.80 100.00 288 0.99 - 0.89 10 10 28.30 100.00 283 0.88 - 0.81 10 10 27.60 100.00 276 0.81 - 0.74 10 10 23.20 100.00 232 0.73 - 0.71 10 10 26.50 100.00 265 0.70 - 0.66 10 10 22.00 100.00 220 0.66 - 0.64 10 10 19.90 100.00 199 0.63 - 0.60 10 10 19.70 100.00 197 --------------------------------------------------------------- 5.92 - 0.60 100 100 23.14 100.00 2314 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:04:19 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.919675 5.917922 5.915311 60.0418 90.0579 59.9999 2272 Reflections read from file xs1714a.hkl; mean (I/sigma) = 31.51 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1116 1211 1117 1152 1722 1519 1511 2272 N (int>3sigma) = 0 1023 1211 1024 1099 1629 1413 1386 2096 Mean intensity = 0.0 51.3 25.2 50.9 55.8 42.0 60.1 58.3 58.2 Mean int/sigma = 0.0 31.0 27.2 30.5 31.1 29.5 32.0 31.5 31.5 Lattice type: P chosen Volume: 146.55 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.918 119.96 90.04 119.96 Niggli form: a.a = 34.990 b.b = 34.991 c.c = 35.022 b.c = -17.481 a.c = -0.025 a.b = -17.474 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.202 [ 2119] Vol = 586.2 Cell: 8.364 8.373 8.370 90.02 89.97 90.04 Volume: 586.20 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.049 RHOMBOHEDRAL R-lattice R(int) = 0.185 [ 1844] Vol = 439.6 Cell: 5.915 5.915 14.503 89.98 90.04 119.96 Volume: 439.65 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.049 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 586] Vol = 439.6 Trigonal Cell: 5.915 5.915 14.503 89.98 90.04 119.96 Volume: 439.65 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.080 TETRAGONAL I-lattice R(int) = 0.163 [ 1875] Vol = 293.1 Cell: 5.919 5.920 8.364 89.95 90.01 90.02 Volume: 293.10 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.054 TETRAGONAL I-lattice R(int) = 0.163 [ 1875] Vol = 293.1 Cell: 5.919 5.920 8.364 89.95 90.01 90.02 Volume: 293.10 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.037 ORTHORHOMBIC I-lattice R(int) = 0.169 [ 1825] Vol = 293.1 Cell: 5.919 8.364 5.920 89.95 89.98 89.99 Volume: 293.10 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.159 [ 1500] Vol = 293.1 Cell: 8.364 5.919 5.920 90.02 90.05 89.99 Volume: 293.10 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.032 MONOCLINIC I-lattice R(int) = 0.153 [ 1512] Vol = 293.1 Cell: 5.918 5.915 8.373 89.98 90.04 89.96 Volume: 293.10 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.053 MONOCLINIC C-lattice R(int) = 0.140 [ 1525] Vol = 293.1 Cell: 8.364 8.373 5.915 89.98 134.97 90.04 Volume: 293.10 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.120 [ 994] Vol = 146.5 Cell: 5.915 5.915 5.918 119.96 90.04 119.96 Volume: 146.55 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1211 0 1516 1519 2272 N (int>3sigma) = 0 0 0 0 1211 0 1392 1413 2096 Mean intensity = 0.0 0.0 0.0 0.0 25.2 0.0 58.8 60.1 58.2 Mean int/sigma = 0.0 0.0 0.0 0.0 27.2 0.0 31.9 32.0 31.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.177 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 23 23 166 530 N I>3s 20 20 125 530 0.7 0.7 0.6 30.0 6.9 6.9 4.1 33.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.202 1972 Fd-3m 1 1 227 C N N N N 37 2284 0.202 2010 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.364370 8.372827 8.370252 90.0151 89.9741 90.0423 ZERR 1.00 0.000303 0.001721 0.003815 0.0022 0.0127 0.0016 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4870284- 606596 548 540 27 20.0 1342948.07 55.14 0.024 0.026 581175- 138065 716 714 27 26.4 242244.13 25.66 0.031 0.039 119392- 41307 611 611 27 22.6 88512.24 10.73 0.044 0.058 11580- 1989 570 568 29 19.6 3981.38 2.73 0.154 0.205 ------------------------------------------------------------------------------------------- 4870284- 1989 2445 2433 110 22.1 392312.64 23.10 0.027 0.030 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 602 590 27 21.9 693664.99 43.16 0.023 0.025 0.016 1.01-0.78 751 751 28 26.8 377277.24 20.78 0.022 0.027 0.028 0.76-0.65 656 656 28 23.4 277124.15 15.34 0.032 0.037 0.041 0.65-0.59 436 436 27 16.1 183728.60 11.63 0.048 0.052 0.058 ------------------------------------------------------------------------------------------------------ inf-0.59 2445 2433 110 22.1 392312.64 23.10 0.027 0.030 0.028 inf-0.60 2324 2312 99 23.4 406378.36 23.82 0.026 0.029 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 590 27 27 100.0 21.9 693664.99 212.15 0.023 0.004 1.01-0.78 751 28 28 100.0 26.8 377277.24 111.93 0.022 0.006 0.76-0.65 656 28 28 100.0 23.4 277124.15 78.85 0.032 0.010 0.65-0.59 436 27 27 100.0 16.1 183728.60 54.82 0.048 0.018 -------------------------------------------------------------------------------------------- inf-0.59 2433 110 110 100.0 22.1 392312.64 117.08 0.027 0.007 inf-0.60 2312 99 99 100.0 23.4 406378.36 121.14 0.026 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:10:41 2018) ID: 2932; threads 39; handles 878; mem 518792.00 (1237700.00)kB; time: 1w 5d 0h 16m 12s MEMORY INFO: Memory PF:0.0, Ph:223.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 697.1, WS: 297.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:223.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.4,peak PF: 697.1, WS: 299.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:10:41 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) 5.91502 ( 0.00080 ) 5.91640 ( 0.00080 ) 5.92265 ( 0.00063 ) 60.05206 ( 0.01261 ) 89.98756 ( 0.00975 ) 60.01743 ( 0.01414 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:10:41 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000014 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.021548 -0.014372 0.007202 ( 0.000003 0.000003 0.000002 ) -0.014372 0.028724 -0.014365 ( 0.000003 0.000004 0.000002 ) 0.007202 -0.014365 0.021562 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(13) 89.988(10) 60.017(14) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 45 | 1.005 ( 0.077) | 0.804 ( 0.035) | 1.278 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 441 | 1.062 ( 0.106) | 1.005 ( 0.290) | 1.297 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 484 peaks identified as outliers and rejected 474 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 474 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 474 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.032 ( 0.144) | 1.122 ( 0.424) | 1.109 ( 0.575) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.275 ( 0.643) | 1.092 ( 0.634) | 1.12- 0.98 | 47 | 1.019 ( 0.102) | 1.057 ( 0.160) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.029 ( 0.093) | 1.035 ( 0.135) | 1.097 ( 0.433) | 0.89- 0.82 | 47 | 1.036 ( 0.085) | 1.007 ( 0.124) | 1.151 ( 0.478) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.196 ( 0.514) | 0.75- 0.71 | 47 | 1.027 ( 0.045) | 0.938 ( 0.113) | 1.296 ( 0.513) | 0.71- 0.67 | 47 | 1.001 ( 0.040) | 0.889 ( 0.071) | 1.260 ( 0.499) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.301 ( 0.513) | 0.63- 0.59 | 51 | 0.945 ( 0.054) | 0.815 ( 0.041) | 1.344 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 474 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.182 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088653 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010206 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116127 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.014 ( 0.108) | 1.028 ( 0.130) | 0.949 ( 0.328) | 0.97- 0.89 | 47 | 1.028 ( 0.089) | 1.029 ( 0.137) | 1.105 ( 0.406) | 0.88- 0.82 | 47 | 1.047 ( 0.079) | 1.022 ( 0.118) | 1.207 ( 0.509) | 0.82- 0.75 | 47 | 1.037 ( 0.080) | 0.987 ( 0.126) | 1.069 ( 0.407) | 0.75- 0.71 | 47 | 1.022 ( 0.044) | 0.934 ( 0.110) | 1.339 ( 0.543) | 0.71- 0.67 | 47 | 0.997 ( 0.043) | 0.885 ( 0.072) | 1.211 ( 0.465) | 0.67- 0.63 | 47 | 0.974 ( 0.047) | 0.841 ( 0.041) | 1.288 ( 0.498) | 0.63- 0.59 | 49 | 0.949 ( 0.045) | 0.812 ( 0.041) | 1.347 ( 0.519) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 472 | 1.014 ( 0.090) | 0.993 ( 0.294) | 1.173 ( 0.533) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb PROFFITPEAK info: 295 peaks in the peak location table UB fit with 132 obs out of 141 (total:141,skipped:0) (93.62%) UB - matrix: -0.069464 0.031056 0.089072 ( 0.000136 0.000152 0.000266 ) -0.069160 -0.065211 -0.010371 ( 0.000130 0.000145 0.000255 ) 0.108808 -0.152982 0.115914 ( 0.000189 0.000211 0.000370 ) M - matrix: 0.021448 -0.014293 0.007142 ( 0.000049 0.000041 0.000054 ) -0.014293 0.028620 -0.014290 ( 0.000041 0.000068 0.000066 ) 0.007142 -0.014290 0.021477 ( 0.000054 0.000066 0.000098 ) unit cell: 5.929(10) 5.923(10) 5.923(12) 60.06(19) 90.02(15) 60.02(18) V = 147.2(4) UB fit with 132 obs out of 141 (total:141,skipped:0) (93.62%) UB - matrix: -0.069464 0.031056 0.089072 ( 0.000136 0.000152 0.000266 ) -0.069160 -0.065211 -0.010371 ( 0.000130 0.000145 0.000255 ) 0.108808 -0.152982 0.115914 ( 0.000189 0.000211 0.000370 ) M - matrix: 0.021448 -0.014293 0.007142 ( 0.000049 0.000041 0.000054 ) -0.014293 0.028620 -0.014290 ( 0.000041 0.000068 0.000066 ) 0.007142 -0.014290 0.021477 ( 0.000054 0.000066 0.000098 ) unit cell: 5.929(10) 5.923(10) 5.923(12) 60.06(19) 90.02(15) 60.02(18) V = 147.2(4) OTKP changes: 25 1 1 1 UB - matrix: -0.069448 0.031184 0.088833 ( 0.000139 0.000156 0.000275 ) -0.068790 -0.065296 -0.009978 ( 0.000128 0.000143 0.000254 ) 0.108924 -0.152829 0.116027 ( 0.000189 0.000212 0.000374 ) M - matrix: 0.021419 -0.014321 0.007155 ( 0.000049 0.000041 0.000054 ) -0.014321 0.028593 -0.014310 ( 0.000041 0.000068 0.000066 ) 0.007155 -0.014310 0.021453 ( 0.000054 0.000066 0.000100 ) UB fit with 134 obs out of 141 (total:141,skipped:0) (95.04%) unit cell: 5.943(10) 5.940(10) 5.933(12) 60.0(2) 89.95(15) 59.90(18) V = 147.9(4) UB fit with 134 obs out of 141 (total:141,skipped:0) (95.04%) UB - matrix: -0.069448 0.031184 0.088833 ( 0.000139 0.000156 0.000275 ) -0.068790 -0.065296 -0.009978 ( 0.000128 0.000143 0.000254 ) 0.108924 -0.152829 0.116027 ( 0.000189 0.000212 0.000374 ) M - matrix: 0.021419 -0.014321 0.007155 ( 0.000049 0.000041 0.000054 ) -0.014321 0.028593 -0.014310 ( 0.000041 0.000068 0.000066 ) 0.007155 -0.014310 0.021453 ( 0.000054 0.000066 0.000100 ) unit cell: 5.943(10) 5.940(10) 5.933(12) 60.0(2) 89.95(15) 59.90(18) V = 147.9(4) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 141 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Run 5 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.089) HKL list info: 261 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069448 0.031184 0.088833 ( 0.000139 0.000156 0.000275 ) -0.068790 -0.065296 -0.009978 ( 0.000128 0.000143 0.000254 ) 0.108924 -0.152829 0.116027 ( 0.000189 0.000212 0.000374 ) M - matrix: 0.021419 -0.014321 0.007155 ( 0.000049 0.000041 0.000054 ) -0.014321 0.028593 -0.014310 ( 0.000041 0.000068 0.000066 ) 0.007155 -0.014310 0.021453 ( 0.000054 0.000066 0.000100 ) UB fit with 134 obs out of 141 (total:141,skipped:0) (95.04%) unit cell: 5.943(10) 5.940(10) 5.933(12) 60.0(2) 89.95(15) 59.90(18) V = 147.9(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 134 obs out of 141 (total:141,skipped:0) (95.04%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb 1 of 101 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 100 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 100 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.48 | 10 | 0.955 ( 0.117) | 0.981 ( 0.163) | 0.969 ( 0.356) | 1.41- 1.12 | 10 | 1.035 ( 0.065) | 1.064 ( 0.091) | 0.952 ( 0.279) | 1.12- 0.97 | 10 | 0.987 ( 0.085) | 0.984 ( 0.105) | 0.971 ( 0.463) | 0.97- 0.92 | 10 | 1.019 ( 0.056) | 1.030 ( 0.128) | 1.152 ( 0.475) | 0.89- 0.82 | 10 | 1.009 ( 0.075) | 0.984 ( 0.110) | 1.116 ( 0.468) | 0.82- 0.76 | 10 | 1.002 ( 0.030) | 0.977 ( 0.097) | 1.133 ( 0.450) | 0.76- 0.70 | 10 | 0.975 ( 0.044) | 0.946 ( 0.050) | 1.286 ( 0.422) | 0.70- 0.67 | 10 | 0.938 ( 0.041) | 0.869 ( 0.061) | 1.323 ( 0.648) | 0.67- 0.63 | 10 | 0.935 ( 0.033) | 0.839 ( 0.025) | 1.577 ( 0.294) | 0.63- 0.59 | 10 | 0.884 ( 0.038) | 0.817 ( 0.028) | 1.444 ( 0.562) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 100 | 0.974 ( 0.078) | 0.949 ( 0.123) | 1.192 ( 0.497) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: -0.069786 0.031303 0.088669 ( 0.000062 0.000072 0.000126 ) -0.068810 -0.065463 -0.010006 ( 0.000045 0.000053 0.000091 ) 0.109087 -0.152709 0.116149 ( 0.000066 0.000078 0.000135 ) M - matrix: 0.021505 -0.014339 0.007171 ( 0.000018 0.000015 0.000021 ) -0.014339 0.028585 -0.014306 ( 0.000015 0.000025 0.000024 ) 0.007171 -0.014306 0.021453 ( 0.000021 0.000024 0.000039 ) unit cell: 5.929(4) 5.939(4) 5.933(5) 59.99(8) 89.98(6) 59.94(7) V = 147.57(18) OTKP changes: 100 1 1 1 UB - matrix: -0.069764 0.031237 0.089002 ( 0.000056 0.000065 0.000113 ) -0.069143 -0.065378 -0.010364 ( 0.000039 0.000046 0.000079 ) 0.109057 -0.153161 0.116288 ( 0.000058 0.000068 0.000118 ) M - matrix: 0.021541 -0.014362 0.007190 ( 0.000016 0.000013 0.000018 ) -0.014362 0.028708 -0.014353 ( 0.000013 0.000022 0.000021 ) 0.007190 -0.014353 0.021552 ( 0.000018 0.000021 0.000034 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 5.920(3) 5.919(3) 5.916(5) 60.04(7) 90.04(5) 60.00(6) V = 146.61(16) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.874) HKL list info: 259 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069764 0.031237 0.089002 ( 0.000056 0.000065 0.000113 ) -0.069143 -0.065378 -0.010364 ( 0.000039 0.000046 0.000079 ) 0.109057 -0.153161 0.116288 ( 0.000058 0.000068 0.000118 ) M - matrix: 0.021541 -0.014362 0.007190 ( 0.000016 0.000013 0.000018 ) -0.014362 0.028708 -0.014353 ( 0.000013 0.000022 0.000021 ) 0.007190 -0.014353 0.021552 ( 0.000018 0.000021 0.000034 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 5.920(3) 5.919(3) 5.916(5) 60.04(7) 90.04(5) 60.00(6) V = 146.61(16) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb 0 of 101 peaks identified as outliers and rejected 101 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 101 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 101 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 10 | 0.958 ( 0.117) | 0.984 ( 0.165) | 0.968 ( 0.355) | 1.41- 1.17 | 10 | 1.019 ( 0.076) | 1.158 ( 0.320) | 1.119 ( 0.476) | 1.12- 0.98 | 10 | 0.996 ( 0.088) | 1.003 ( 0.118) | 0.932 ( 0.447) | 0.97- 0.92 | 10 | 1.033 ( 0.053) | 1.058 ( 0.111) | 1.074 ( 0.423) | 0.92- 0.82 | 10 | 1.002 ( 0.070) | 0.962 ( 0.106) | 1.180 ( 0.516) | 0.82- 0.76 | 10 | 1.013 ( 0.043) | 0.984 ( 0.100) | 1.104 ( 0.440) | 0.76- 0.71 | 10 | 0.983 ( 0.049) | 0.968 ( 0.068) | 1.342 ( 0.409) | 0.70- 0.67 | 10 | 0.947 ( 0.043) | 0.878 ( 0.065) | 1.348 ( 0.633) | 0.67- 0.63 | 10 | 0.939 ( 0.030) | 0.849 ( 0.027) | 1.511 ( 0.391) | 0.62- 0.59 | 11 | 0.891 ( 0.029) | 0.821 ( 0.024) | 1.462 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 101 | 0.977 ( 0.078) | 0.965 ( 0.166) | 1.207 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 190 | 1.116 ( 0.112) | 1.228 ( 0.438) | 1.169 ( 0.595) | 13.3-19.0 | 190 | 1.081 ( 0.056) | 1.139 ( 0.295) | 1.198 ( 0.523) | 19.0-23.1 | 190 | 1.069 ( 0.071) | 1.141 ( 0.377) | 1.176 ( 0.496) | 23.1-27.2 | 190 | 1.035 ( 0.079) | 1.080 ( 0.285) | 1.188 ( 0.569) | 27.2-30.8 | 190 | 1.013 ( 0.074) | 1.011 ( 0.254) | 1.197 ( 0.510) | 30.8-33.8 | 190 | 0.985 ( 0.082) | 0.925 ( 0.096) | 1.197 ( 0.509) | 33.8-36.9 | 190 | 0.965 ( 0.076) | 0.902 ( 0.096) | 1.176 ( 0.490) | 36.9-39.7 | 190 | 0.950 ( 0.090) | 0.871 ( 0.136) | 1.198 ( 0.557) | 39.7-42.7 | 190 | 0.929 ( 0.075) | 0.838 ( 0.081) | 1.204 ( 0.516) | 42.7-49.9 | 189 | 0.934 ( 0.085) | 0.814 ( 0.065) | 1.154 ( 0.467) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 1899 | 1.008 ( 0.103) | 0.995 ( 0.284) | 1.186 ( 0.525) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0097 b=1.26 e3 dimension: a=0.0020 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:11:02 2018 PROFFITMAIN - Started at Tue Mar 27 15:11:02 2018 OTKP changes: 1899 2 4 5 OTKP changes: 1899 2 4 5 UB - matrix: -0.070145 0.031132 0.088923 ( 0.000011 0.000013 0.000012 ) -0.068725 -0.065922 -0.010395 ( 0.000011 0.000013 0.000012 ) 0.109147 -0.153015 0.116320 ( 0.000010 0.000011 0.000010 ) M - matrix: 0.021556 -0.014354 0.007173 ( 0.000003 0.000002 0.000002 ) -0.014354 0.028729 -0.014345 ( 0.000002 0.000004 0.000002 ) 0.007173 -0.014345 0.021546 ( 0.000002 0.000002 0.000003 ) UB fit with 1899 obs out of 1899 (total:1899,skipped:0) (100.00%) unit cell: 5.9141(7) 5.9127(7) 5.9144(6) 60.047(11) 90.021(9) 60.027(12) V = 146.38(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070042 0.030658 0.088969 ( 0.000029 0.000028 0.000016 ) -0.068254 -0.066139 -0.010492 ( 0.000026 0.000025 0.000015 ) 0.109064 -0.153048 0.115959 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021459 -0.014325 0.007131 ( 0.000008 0.000006 0.000004 ) -0.014325 0.028738 -0.014326 ( 0.000006 0.000008 0.000005 ) 0.007131 -0.014326 0.021472 ( 0.000004 0.000005 0.000004 ) unit cell: 5.9276(14) 5.9138(14) 5.9251(11) 60.01(2) 89.962(18) 60.00(2) V = 146.95(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070337 0.030940 0.088804 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066138 -0.010672 ( 0.000024 0.000023 0.000013 ) 0.109337 -0.153285 0.116366 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021581 -0.014412 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028828 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014384 0.021541 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9075(13) 5.9182(10) 60.05(2) 90.064(16) 60.00(2) V = 146.26(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.791) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070337 0.030940 0.088804 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066138 -0.010672 ( 0.000024 0.000023 0.000013 ) 0.109337 -0.153285 0.116366 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021581 -0.014412 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028828 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014384 0.021541 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9075(13) 5.9182(10) 60.05(2) 90.064(16) 60.00(2) V = 146.26(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070337 0.030940 0.088804 ( 0.000026 0.000026 0.000015 ) -0.068404 -0.066138 -0.010672 ( 0.000024 0.000023 0.000013 ) 0.109337 -0.153285 0.116366 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021581 -0.014412 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014412 0.028828 -0.014384 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014384 0.021541 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9157(13) 5.9075(13) 5.9182(10) 60.05(2) 90.064(16) 60.00(2) V = 146.26(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070407 0.031355 0.088641 ( 0.000026 0.000022 0.000028 ) -0.068572 -0.066009 -0.010225 ( 0.000031 0.000027 0.000033 ) 0.108985 -0.152626 0.116243 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021537 -0.014315 0.007129 ( 0.000007 0.000005 0.000005 ) -0.014315 0.028635 -0.014288 ( 0.000005 0.000007 0.000005 ) 0.007129 -0.014288 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(17) 5.9212(16) 5.9221(13) 60.03(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070364 0.031217 0.088839 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065851 -0.010360 ( 0.000030 0.000026 0.000032 ) 0.109163 -0.153145 0.116582 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021600 -0.014384 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028764 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014399 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9094(16) 5.9163(16) 5.9142(12) 59.95(2) 89.952(19) 60.01(3) V = 146.16(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.791) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070364 0.031217 0.088839 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065851 -0.010360 ( 0.000030 0.000026 0.000032 ) 0.109163 -0.153145 0.116582 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021600 -0.014384 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028764 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014399 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9094(16) 5.9163(16) 5.9142(12) 59.95(2) 89.952(19) 60.01(3) V = 146.16(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070364 0.031217 0.088839 ( 0.000023 0.000020 0.000025 ) -0.068793 -0.065851 -0.010360 ( 0.000030 0.000026 0.000032 ) 0.109163 -0.153145 0.116582 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021600 -0.014384 0.007188 ( 0.000007 0.000005 0.000005 ) -0.014384 0.028764 -0.014399 ( 0.000005 0.000006 0.000005 ) 0.007188 -0.014399 0.021591 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9094(16) 5.9163(16) 5.9142(12) 59.95(2) 89.952(19) 60.01(3) V = 146.16(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) UB - matrix: -0.070169 0.031459 0.088647 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065706 -0.010198 ( 0.000021 0.000032 0.000027 ) 0.108915 -0.152879 0.116142 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021528 -0.014334 0.007132 ( 0.000005 0.000005 0.000004 ) -0.014334 0.028679 -0.014297 ( 0.000005 0.000009 0.000005 ) 0.007132 -0.014297 0.021451 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9183(15) 5.9193(15) 5.9265(11) 60.03(2) 89.944(18) 59.99(3) V = 146.91(5) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 UB - matrix: -0.070136 0.031449 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068732 -0.066014 -0.009954 ( 0.000018 0.000028 0.000024 ) 0.109182 -0.153122 0.116570 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021564 -0.014387 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014387 0.028793 -0.014397 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014397 0.021589 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9136(14) 5.9129(11) 59.97(2) 89.935(17) 59.97(2) V = 146.22(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.791) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070136 0.031449 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068732 -0.066014 -0.009954 ( 0.000018 0.000028 0.000024 ) 0.109182 -0.153122 0.116570 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021564 -0.014387 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014387 0.028793 -0.014397 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014397 0.021589 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9136(14) 5.9129(11) 59.97(2) 89.935(17) 59.97(2) V = 146.22(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070136 0.031449 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068732 -0.066014 -0.009954 ( 0.000018 0.000028 0.000024 ) 0.109182 -0.153122 0.116570 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021564 -0.014387 0.007177 ( 0.000005 0.000005 0.000004 ) -0.014387 0.028793 -0.014397 ( 0.000005 0.000008 0.000005 ) 0.007177 -0.014397 0.021589 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9159(13) 5.9136(14) 5.9129(11) 59.97(2) 89.935(17) 59.97(2) V = 146.22(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) UB - matrix: -0.070038 0.031445 0.088817 ( 0.000058 0.000068 0.000118 ) -0.068848 -0.065637 -0.010176 ( 0.000068 0.000080 0.000138 ) 0.109315 -0.153104 0.116520 ( 0.000066 0.000077 0.000134 ) M - matrix: 0.021595 -0.014420 0.007218 ( 0.000019 0.000016 0.000021 ) -0.014420 0.028738 -0.014379 ( 0.000016 0.000026 0.000025 ) 0.007218 -0.014379 0.021569 ( 0.000021 0.000025 0.000038 ) unit cell: 5.919(5) 5.923(5) 5.916(5) 60.02(9) 90.01(7) 59.91(9) V = 146.5(2) OTKP changes: 101 1 1 1 UB - matrix: -0.069784 0.031261 0.089005 ( 0.000055 0.000065 0.000112 ) -0.069115 -0.065427 -0.010371 ( 0.000066 0.000077 0.000133 ) 0.109084 -0.153175 0.116290 ( 0.000058 0.000068 0.000117 ) M - matrix: 0.021546 -0.014369 0.007191 ( 0.000017 0.000014 0.000019 ) -0.014369 0.028721 -0.014352 ( 0.000014 0.000023 0.000022 ) 0.007191 -0.014352 0.021553 ( 0.000019 0.000022 0.000034 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 5.920(5) 5.917(5) 5.915(5) 60.06(9) 90.04(7) 59.99(8) V = 146.54(18) Run 5 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.866) HKL list info: 253 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069784 0.031261 0.089005 ( 0.000055 0.000065 0.000112 ) -0.069115 -0.065427 -0.010371 ( 0.000066 0.000077 0.000133 ) 0.109084 -0.153175 0.116290 ( 0.000058 0.000068 0.000117 ) M - matrix: 0.021546 -0.014369 0.007191 ( 0.000017 0.000014 0.000019 ) -0.014369 0.028721 -0.014352 ( 0.000014 0.000023 0.000022 ) 0.007191 -0.014352 0.021553 ( 0.000019 0.000022 0.000034 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 5.920(5) 5.917(5) 5.915(5) 60.06(9) 90.04(7) 59.99(8) V = 146.54(18) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 5) ******* UB - matrix: 0.146780 -0.097883 0.048985 ( 0.000043 0.000050 0.000087 ) -0.000004 0.138346 -0.069078 ( 0.000054 0.000064 0.000110 ) 0.000000 -0.000002 0.119921 ( 0.000077 0.000090 0.000156 ) M - matrix: 0.021544 -0.014368 0.007190 ( 0.000013 0.000011 0.000016 ) -0.014368 0.028721 -0.014352 ( 0.000011 0.000020 0.000021 ) 0.007190 -0.014352 0.021552 ( 0.000016 0.000021 0.000041 ) UB fit with 101 obs out of 101 (total:101,skipped:0) (100.00%) unit cell: 5.920(2) 5.917(4) 5.915(8) 60.06(11) 90.04(6) 59.99(6) V = 146.5(2) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.070020 0.031108 0.088880 ( 0.000012 0.000013 0.000012 ) -0.068728 -0.065803 -0.010442 ( 0.000013 0.000015 0.000014 ) 0.109184 -0.153070 0.116416 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021547 -0.014368 0.007205 ( 0.000003 0.000002 0.000002 ) -0.014368 0.028728 -0.014368 ( 0.000002 0.000004 0.000002 ) 0.007205 -0.014368 0.021561 ( 0.000002 0.000002 0.000003 ) UB fit with 1899 obs out of 1899 (total:1899,skipped:0) (100.00%) unit cell: 5.9189(8) 5.9167(8) 5.9158(6) 60.040(12) 90.076(10) 60.021(14) V = 146.53(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 62 reflections under beam stop or inside a detector rejection region 17 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof 2589 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:11:06 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.791) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.791) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.791) Run 5 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.866) PROFFIT INFO: signal sum: min=249.0000 max=20926870.0000 PROFFIT INFO: signal sum lp corr: min=451.5611 max=2971554.0368 PROFFIT INFO: background sum: min=578.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=722.4977 max=4754486.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47806.8789 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=248.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 21 112 254 528 593 1030 1713 2362 2589 Percent 0.0 0.0 0.8 4.3 9.8 20.4 22.9 39.8 66.2 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2589 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2589 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4754487- 1212101 258 1951364.19 120.89 100.00 1211300- 689409 258 916436.92 106.77 100.00 688486- 281650 258 450741.72 97.09 100.00 281474- 178050 258 216479.85 74.13 100.00 177808- 132130 258 156274.47 52.12 100.00 132117- 100416 258 113960.99 37.02 100.00 100377- 74587 258 88471.91 30.34 100.00 74578- 5891 258 42342.24 20.15 100.00 5849- 3184 258 4219.23 5.48 97.67 3179- 722 267 2344.15 3.88 60.30 ------------------------------------------------------------------------------------ 4754487- 722 2589 392901.16 54.61 95.67 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 258 731904.79 88.63 98.84 1.28- 1.05 258 561605.72 67.43 97.67 1.05- 0.92 258 493350.88 63.36 98.06 0.92- 0.82 258 351897.43 52.99 95.74 0.82- 0.74 258 437917.55 58.88 97.29 0.74- 0.67 258 392018.28 57.43 96.51 0.67- 0.61 258 226208.33 40.33 94.96 0.61- 0.56 258 315397.48 46.88 92.25 0.56- 0.51 258 228870.83 38.10 91.09 0.51- 0.40 267 196685.07 32.83 94.38 ------------------------------------------------------------------------------------ 5.26- 0.40 2589 392901.16 54.61 95.67 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:11:07 2018 Sorting 2589 observations 288 unique observations with > 7.00 F2/sig(F2) 2589 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 24 445 Total number of frames 445 Maximum number of 288 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2589 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 12 226 Total number of frames 226 2084 observations > 7.00 F2/sig(F2) 2084 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 12 226 Total number of frames 226 Removing 'redundancy=1' reflections Average redundancy: 7.6 (Out of 2084 removed 36 = 2048, unique = 268) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2048 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 12 226 Total number of frames 226 268 unique data precomputed (should be 268) 268 unique data with 2048 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.6 (Out of 2048 removed 0 = 2048, unique = 268) 268 unique data precomputed (should be 268) 268 unique data with 2048 observations RMS deviation of equivalent data = 0.71912 Rint = 0.68991 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.66874, wR= 3.52801 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68355, wR= 2.88959, Acormin=0.116, Acormax=1.797, Acor_av=0.816 F test: Probability=0.000, F= 0.954 Trying model 2 (ne=2, no=1)... Results: Rint= 0.83429, wR= 2.75613, Acormin=-0.527, Acormax=1.738, Acor_av=0.523 F test: Probability=0.000, F= 0.640 Trying model 3 (ne=4, no=0)... Results: Rint= 0.71855, wR= 2.55420, Acormin=-0.046, Acormax=2.136, Acor_av=0.698 F test: Probability=0.000, F= 0.859 Trying model 4 (ne=4, no=1)... Results: Rint= 0.86621, wR= 2.45135, Acormin=-0.467, Acormax=1.866, Acor_av=0.430 F test: Probability=0.000, F= 0.590 Trying model 5 (ne=4, no=3)... Results: Rint= 0.92420, wR= 2.32855, Acormin=-1.235, Acormax=1.695, Acor_av=0.260 F test: Probability=0.000, F= 0.516 Trying model 6 (ne=6, no=0)... Results: Rint= 0.74460, wR= 2.52966, Acormin=-0.263, Acormax=2.598, Acor_av=0.623 F test: Probability=0.000, F= 0.794 Trying model 7 (ne=6, no=1)... Results: Rint= 0.87528, wR= 2.51271, Acormin=-0.642, Acormax=2.116, Acor_av=0.375 F test: Probability=0.000, F= 0.574 Trying model 8 (ne=6, no=3)... Results: Rint= 0.92681, wR= 2.31701, Acormin=-1.478, Acormax=1.701, Acor_av=0.227 F test: Probability=0.000, F= 0.510 Trying model 9 (ne=6, no=5)... Results: Rint= 0.92641, wR= 2.30956, Acormin=-1.816, Acormax=1.858, Acor_av=0.191 F test: Probability=0.000, F= 0.507 Trying model 10 (ne=8, no=0)... Results: Rint= 0.84779, wR= 2.34722, Acormin=-0.627, Acormax=2.204, Acor_av=0.411 F test: Probability=0.000, F= 0.607 Trying model 11 (ne=8, no=1)... Results: Rint= 0.98006, wR= 1.86979, Acormin=-1.279, Acormax=1.407, Acor_av=0.125 F test: Probability=0.000, F= 0.453 Trying model 12 (ne=8, no=3)... Results: Rint= 1.00130, wR= 1.58303, Acormin=-0.050, Acormax=0.069, Acor_av=0.002 F test: Probability=0.000, F= 0.432 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99971, wR= 1.61880, Acormin=-0.046, Acormax=0.074, Acor_av=0.002 F test: Probability=0.000, F= 0.431 Trying model 14 (ne=8, no=7)... Results: Rint= 1.01210, wR= 1.67830, Acormin=-0.045, Acormax=0.070, Acor_av=0.002 F test: Probability=0.000, F= 0.417 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.85943 There are 226 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 230 pars with 26565 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.71912 Using Levenberg-Marquardt: 0.00010 New wR= 0.69416 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.68991 with corrections 0.66257 Rint for all data: 0.85943 with corrections 0.83741 12 observations identified as outliers and rejected Cycle 2 wR= 0.66867 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.66679 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66874 with corrections 0.64637 Rint for all data: 0.85943 with corrections 0.84299 10 observations identified as outliers and rejected Cycle 3 wR= 0.64722 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64543 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65791 with corrections 0.63823 Rint for all data: 0.85943 with corrections 0.84595 10 observations identified as outliers and rejected Cycle 4 wR= 0.62604 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62455 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65265 with corrections 0.63678 Rint for all data: 0.85943 with corrections 0.84793 8 observations identified as outliers and rejected Cycle 5 wR= 0.61086 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.60796 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.64908 with corrections 0.63707 Rint for all data: 0.85943 with corrections 0.85006 5 observations identified as outliers and rejected Final wR= 0.60796 Final frame scales: Min= 0.7064 Max= 2.5472 Final absorption correction factors: Amin= 0.4003 Amax= 1.5485 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=719.3522 max=6017358.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=128.7600 max=76351.6875 PROFFIT INFO: 1 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/108 2588 reflections read from tmp file 1960 reflections are rejected (1892 as outliers, 68 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9+ Number of groups: 0 98 42 26 19 9 5 0 2 Initial Chi^2= 0.53303 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.84041 Current error model SIG(F2)^2 = 202.71*I_RAW + 0.00*I_BACK+(0.02249*)^2 Cycle 2, Chi^2= 1.00250 Current error model SIG(F2)^2 = 176.74*I_RAW + 0.00*I_BACK+(0.01857*)^2 Cycle 3, Chi^2= 0.99959 Current error model SIG(F2)^2 = 176.02*I_RAW + 0.00*I_BACK+(0.01896*)^2 Cycle 4, Chi^2= 1.00010 Current error model SIG(F2)^2 = 176.22*I_RAW + 0.00*I_BACK+(0.01887*)^2 Cycle 5, Chi^2= 0.99998 Current error model SIG(F2)^2 = 176.17*I_RAW + 0.00*I_BACK+(0.01889*)^2 Final Chi^2= 0.99998 Final error model SIG(F2)^2 = 176.17*I_RAW + 0.00*I_BACK+(0.01889*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 6017359- 1219271 258 2025669.33 101.10 100.00 1206720- 600784 258 864134.60 53.75 100.00 600214- 277889 258 417607.40 46.94 100.00 277878- 176555 258 218984.95 34.56 100.00 176295- 129788 258 149793.19 24.63 100.00 129682- 93609 258 112276.75 18.83 100.00 93541- 63046 258 77439.98 14.81 100.00 62781- 6146 258 36480.87 10.90 96.12 6127- 2905 258 3978.70 3.68 72.87 2902- 719 266 2115.08 2.85 39.47 ------------------------------------------------------------------------------------ 6017359- 719 2588 389646.44 31.12 90.69 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 258 847931.00 64.99 96.90 1.28- 1.05 258 590402.76 45.61 95.35 1.05- 0.92 258 537570.44 37.82 94.57 0.92- 0.82 258 354368.75 29.34 89.15 0.82- 0.74 258 430626.29 29.33 93.80 0.74- 0.67 258 363307.80 28.16 90.31 0.67- 0.61 258 202273.52 20.08 85.66 0.61- 0.56 258 277206.98 21.86 87.60 0.56- 0.51 258 174120.65 18.62 84.50 0.51- 0.40 266 126806.25 15.85 89.10 ------------------------------------------------------------------------------------ 5.26- 0.40 2588 389646.44 31.12 90.69 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.28 258 847931.00 64.99 96.90 5.26- 1.05 516 719166.88 55.30 96.12 5.26- 0.92 774 658634.73 49.47 95.61 5.26- 0.82 1032 582568.24 44.44 93.99 5.26- 0.74 1290 552179.85 41.42 93.95 5.26- 0.67 1548 520701.17 39.21 93.35 5.26- 0.61 1806 475211.51 36.48 92.25 5.26- 0.56 2064 450460.94 34.65 91.67 5.26- 0.51 2322 419756.47 32.87 90.87 5.26- 0.40 2588 389646.44 31.12 90.69 ------------------------------------------------------------------------------------ 5.26- 0.40 2588 389646.44 31.12 90.69 Scale applied to data: s=0.166186 (maximum obs:6017358.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.850; Rsigma 0.021: data 2588 -> merged 313 With outlier rejection... Rint 0.774; Rsigma 0.021: data 2404 -> merged 313 Rejected total: 184, method kkm 169, method Blessing 15 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404346, 5.272023 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 11.53 100.00 173 1.46 - 1.12 15 15 18.13 100.00 272 1.08 - 0.96 15 15 16.00 100.00 240 0.96 - 0.86 15 15 14.13 100.00 212 0.86 - 0.79 15 15 12.87 100.00 193 0.79 - 0.73 15 15 10.73 100.00 161 0.73 - 0.69 15 15 9.87 100.00 148 0.69 - 0.65 15 15 10.60 100.00 159 0.65 - 0.63 15 15 6.13 100.00 92 0.63 - 0.60 21 21 7.00 100.00 147 --------------------------------------------------------------- 5.92 - 0.60 156 156 11.52 100.00 1797 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:11:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918875 5.916661 5.915847 60.0398 90.0760 60.0215 2403 Reflections read from file xs1714a.hkl; mean (I/sigma) = 30.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1180 1279 1191 1216 1825 1608 1595 2403 N (int>3sigma) = 0 1063 1279 1074 1134 1708 1471 1438 2179 Mean intensity = 0.0 55.7 26.5 55.1 59.8 45.3 63.4 61.0 61.6 Mean int/sigma = 0.0 30.5 26.1 29.9 30.3 28.8 31.3 30.6 30.6 Lattice type: P chosen Volume: 146.53 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.917 119.96 90.05 119.95 Niggli form: a.a = 34.987 b.b = 34.997 c.c = 35.007 b.c = -17.480 a.c = -0.028 a.b = -17.471 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.209 [ 2249] Vol = 586.1 Cell: 8.363 8.374 8.370 90.00 89.98 90.03 Volume: 586.13 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.057 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 1972] Vol = 439.6 Cell: 5.916 5.915 14.499 89.97 90.06 119.95 Volume: 439.60 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.057 RHOMBOHEDRAL R-lattice R(int) = 0.187 [ 626] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.499 89.97 90.06 119.95 Volume: 439.60 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.063 TETRAGONAL I-lattice R(int) = 0.171 [ 2006] Vol = 293.1 Cell: 5.920 5.920 8.363 89.97 90.01 90.03 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.050 TETRAGONAL I-lattice R(int) = 0.171 [ 2006] Vol = 293.1 Cell: 5.920 5.920 8.363 89.97 90.01 90.03 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 1957] Vol = 293.1 Cell: 5.920 8.363 5.920 89.97 89.97 89.99 Volume: 293.06 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.015 MONOCLINIC I-lattice R(int) = 0.160 [ 1629] Vol = 293.1 Cell: 8.363 5.920 5.920 90.03 90.03 89.99 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.036 MONOCLINIC I-lattice R(int) = 0.161 [ 1636] Vol = 293.1 Cell: 5.917 5.915 8.374 89.98 90.02 89.95 Volume: 293.06 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.038 MONOCLINIC C-lattice R(int) = 0.143 [ 1653] Vol = 293.1 Cell: 8.363 8.374 5.915 89.98 134.97 90.03 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.124 [ 1096] Vol = 146.5 Cell: 5.915 5.916 5.917 119.96 90.05 119.95 Volume: 146.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1279 0 1610 1608 2403 N (int>3sigma) = 0 0 0 0 1279 0 1459 1471 2179 Mean intensity = 0.0 0.0 0.0 0.0 26.5 0.0 62.2 63.4 61.6 Mean int/sigma = 0.0 0.0 0.0 0.0 26.1 0.0 31.0 31.3 30.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.165 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 22 22 170 563 N I>3s 19 19 119 563 0.7 0.7 0.6 31.9 6.4 6.4 3.9 32.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.209 2098 Fd-3m 1 1 227 C N N N N 37 2284 0.210 2136 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362860 8.373961 8.369626 90.0012 89.9839 90.0293 ZERR 1.00 0.000297 0.001700 0.003751 0.0020 0.0125 0.0015 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3287525- 634710 476 450 31 14.5 968148.41 57.30 0.711 0.726 626677- 457841 335 330 31 10.6 526647.56 40.02 0.897 0.860 450665- 348831 275 264 31 8.5 364130.45 32.90 0.870 0.798 346692- 284310 297 271 31 8.7 259613.03 26.28 0.897 0.971 278408- 204797 258 223 31 7.2 200273.18 23.57 0.822 0.838 202571- 145932 251 222 31 7.2 136717.79 21.80 0.667 0.764 145644- 91004 285 270 31 8.7 96861.88 16.61 0.574 0.621 90989- 59709 156 144 31 4.6 70793.71 14.11 0.453 0.285 59353- 46147 144 130 31 4.2 54624.60 12.41 0.448 0.294 44475- 1590 111 100 34 2.9 23941.08 7.41 0.639 0.586 ------------------------------------------------------------------------------------------- 3287525- 1590 2588 2404 313 7.7 373045.19 30.69 0.774 0.771 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 494 469 31 15.1 724512.72 56.11 0.770 0.836 0.013 1.05-0.83 469 454 31 14.6 455274.59 34.34 0.860 0.998 0.019 0.83-0.72 373 355 31 11.5 356338.45 27.13 0.771 0.798 0.025 0.72-0.65 345 320 34 9.4 258070.77 23.84 0.780 0.787 0.027 0.64-0.60 244 221 31 7.1 238797.72 20.71 0.781 0.835 0.031 0.59-0.56 211 194 33 5.9 166717.64 17.65 0.635 0.622 0.036 0.56-0.52 158 139 31 4.5 178205.78 19.22 0.579 0.628 0.035 0.52-0.49 144 122 33 3.7 133400.43 15.96 0.708 0.597 0.036 0.49-0.45 90 76 31 2.5 133126.55 16.10 0.328 0.229 0.040 0.45-0.40 60 54 27 2.0 91594.54 14.02 0.231 0.166 0.045 ------------------------------------------------------------------------------------------------------ inf-0.40 2588 2404 313 7.7 373045.19 30.69 0.774 0.771 0.021 inf-0.60 1902 1798 156 11.5 447574.99 35.21 0.795 0.859 0.019 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 469 31 31 100.0 15.1 724512.72 256.00 0.770 0.004 1.05-0.83 454 31 31 100.0 14.6 455274.59 158.19 0.860 0.007 0.83-0.72 355 31 31 100.0 11.5 356338.45 115.83 0.771 0.011 0.72-0.65 320 34 34 100.0 9.4 258070.77 91.77 0.780 0.013 0.64-0.60 221 31 31 100.0 7.1 238797.72 71.43 0.781 0.015 0.59-0.56 194 36 33 91.7 5.9 166717.64 53.16 0.635 0.017 0.56-0.52 139 34 31 91.2 4.5 178205.78 52.46 0.579 0.018 0.52-0.49 122 48 33 68.8 3.7 133400.43 40.58 0.708 0.024 0.49-0.45 76 61 31 50.8 2.5 133126.55 28.79 0.328 0.027 0.45-0.40 54 126 27 21.4 2.0 91594.54 21.73 0.231 0.032 -------------------------------------------------------------------------------------------- inf-0.40 2404 464 313 67.5 7.7 373045.19 126.49 0.774 0.012 inf-0.60 1798 156 156 100.0 11.5 447574.99 153.89 0.795 0.008 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: -0.024983 -0.079449 -0.015554 ( 0.000007 0.000007 0.000007 ) 0.072487 -0.029142 0.032901 ( 0.000007 0.000008 0.000007 ) -0.036265 -0.003616 0.076534 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007194 0.000004 -0.000002 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007175 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000002 0.000000 0.007182 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.024983 -0.079449 -0.015554 ( 0.000007 0.000007 0.000007 ) 0.072487 -0.029142 0.032901 ( 0.000007 0.000008 0.000007 ) -0.036265 -0.003616 0.076534 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3629(7) 8.3740(7) 8.3697(5) 90.001(6) 89.984(6) 90.029(7) V = 586.13(8) unit cell: 8.3689(2) 8.3689(2) 8.3689(2) 90.0 90.0 90.0 V = 586.13(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.791) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.791) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.791) Run 5 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.866) PROFFIT INFO: signal sum: min=249.0000 max=20926870.0000 PROFFIT INFO: signal sum lp corr: min=451.5611 max=2971554.0368 PROFFIT INFO: background sum: min=578.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=722.4977 max=4754486.5000 PROFFIT INFO: sig(Inet): min=128.9277 max=47806.8789 PROFFIT INFO: Inet/sig(Inet): min=1.01 max=248.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 42 224 508 1056 1186 2060 3426 4724 5178 Percent 0.0 0.0 0.8 4.3 9.8 20.4 22.9 39.8 66.2 91.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2589 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2589 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4754487- 1212101 258 1951364.19 120.89 100.00 1211300- 689409 258 916436.92 106.77 100.00 688486- 281650 258 450741.72 97.09 100.00 281474- 178050 258 216479.85 74.13 100.00 177808- 132130 258 156274.47 52.12 100.00 132117- 100416 258 113960.99 37.02 100.00 100377- 74587 258 88471.91 30.34 100.00 74578- 5891 258 42342.24 20.15 100.00 5849- 3184 258 4219.23 5.48 97.67 3179- 722 267 2344.15 3.88 60.30 ------------------------------------------------------------------------------------ 4754487- 722 2589 392901.16 54.61 95.67 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 258 772195.48 96.11 99.61 1.39- 1.12 258 741028.90 64.10 100.00 1.12- 0.96 258 447070.89 69.71 97.67 0.96- 0.88 258 380347.01 61.88 96.12 0.88- 0.81 258 483159.94 70.88 99.22 0.81- 0.73 258 258712.96 42.29 98.45 0.73- 0.71 258 182561.13 34.06 86.05 0.71- 0.65 258 343356.64 50.51 96.12 0.65- 0.62 258 166919.36 28.79 88.76 0.62- 0.58 267 161723.63 28.67 94.76 ------------------------------------------------------------------------------------ 4.82- 0.58 2589 392901.16 54.61 95.67 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:11:08 2018 Sorting 2589 observations 85 unique observations with > 7.00 F2/sig(F2) 2589 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 24 445 Total number of frames 445 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2589 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 4 77 Total number of frames 77 2084 observations > 7.00 F2/sig(F2) 2084 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 4 77 Total number of frames 77 Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2084 removed 3 = 2081, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2081 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 4 77 Total number of frames 77 93 unique data precomputed (should be 93) 93 unique data with 2081 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2081 removed 0 = 2081, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2081 observations RMS deviation of equivalent data = 0.19528 Rint = 0.13392 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.12756, wR= 0.18891 Trying model 1 (ne=2, no=0)... Results: Rint= 0.09860, wR= 0.13621, Acormin=0.731, Acormax=1.309, Acor_av=0.956 F test: Probability=1.000, F= 1.669 Trying model 2 (ne=2, no=1)... Results: Rint= 0.09797, wR= 0.13041, Acormin=0.649, Acormax=1.367, Acor_av=0.875 F test: Probability=0.599, F= 1.011 Trying model 3 (ne=4, no=0)... Results: Rint= 0.08448, wR= 0.11590, Acormin=0.653, Acormax=1.436, Acor_av=0.917 F test: Probability=1.000, F= 1.356 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08062, wR= 0.10837, Acormin=0.517, Acormax=1.385, Acor_av=0.811 F test: Probability=0.979, F= 1.096 Trying model 5 (ne=4, no=3)... Results: Rint= 0.06972, wR= 0.09906, Acormin=0.428, Acormax=1.403, Acor_av=0.790 F test: Probability=1.000, F= 1.332 Trying model 6 (ne=6, no=0)... Results: Rint= 0.07800, wR= 0.10956, Acormin=0.691, Acormax=1.460, Acor_av=0.923 F test: Probability=0.000, F= 0.798 Trying model 7 (ne=6, no=1)... Results: Rint= 0.07376, wR= 0.10253, Acormin=0.515, Acormax=1.466, Acor_av=0.811 F test: Probability=0.000, F= 0.891 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06486, wR= 0.09437, Acormin=0.436, Acormax=1.490, Acor_av=0.801 F test: Probability=0.999, F= 1.148 Trying model 9 (ne=6, no=5)... Results: Rint= 0.06412, wR= 0.08947, Acormin=0.306, Acormax=1.295, Acor_av=0.698 F test: Probability=0.648, F= 1.017 Trying model 10 (ne=8, no=0)... Results: Rint= 0.07653, wR= 0.10568, Acormin=0.591, Acormax=1.467, Acor_av=0.851 F test: Probability=0.000, F= 0.716 Trying model 11 (ne=8, no=1)... Results: Rint= 0.06673, wR= 0.09350, Acormin=0.513, Acormax=1.564, Acor_av=0.835 F test: Probability=0.000, F= 0.940 Trying model 12 (ne=8, no=3)... Results: Rint= 0.06320, wR= 0.08979, Acormin=0.259, Acormax=0.717, Acor_av=0.393 F test: Probability=0.827, F= 1.044 Trying model 13 (ne=8, no=5)... Results: Rint= 0.05526, wR= 0.08018, Acormin=0.277, Acormax=0.877, Acor_av=0.446 F test: Probability=1.000, F= 1.358 Trying model 14 (ne=8, no=7)... Results: Rint= 0.04917, wR= 0.07263, Acormin=0.299, Acormax=0.996, Acor_av=0.478 F test: Probability=1.000, F= 1.702 Final absorption model (ne=6, no=3): Rint= 0.06486, Acormin=0.436, Acormax=1.490, Acor_av=0.801 Combined refinement in use Rint: 0.13405 There are 77 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 113 pars with 6441 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.19528 Using Levenberg-Marquardt: 0.00010 New wR= 0.05922 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.13392 with corrections 0.04708 Rint for all data: 0.13405 with corrections 0.04729 0 observations identified as outliers and rejected Cycle 2 wR= 0.05922 Using Levenberg-Marquardt: 0.00001 New wR= 0.05311 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.13392 with corrections 0.04132 Rint for all data: 0.13405 with corrections 0.04153 0 observations identified as outliers and rejected Cycle 3 wR= 0.05311 Using Levenberg-Marquardt: 0.00000 New wR= 0.05215 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.13392 with corrections 0.04036 Rint for all data: 0.13405 with corrections 0.04057 0 observations identified as outliers and rejected Cycle 4 wR= 0.05215 Using Levenberg-Marquardt: 0.00000 New wR= 0.05168 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.13392 with corrections 0.03989 Rint for all data: 0.13405 with corrections 0.04011 0 observations identified as outliers and rejected Cycle 5 wR= 0.05168 Using Levenberg-Marquardt: 0.00000 New wR= 0.05139 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.13392 with corrections 0.03961 Rint for all data: 0.13405 with corrections 0.03983 0 observations identified as outliers and rejected Final wR= 0.05139 Final frame scales: Min= 0.7584 Max= 1.3691 Final absorption correction factors: Amin= 0.5886 Amax= 1.3951 PROFFIT INFO: Inet (after scale3 abspack): min=859.3578 max=5619657.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=128.5902 max=59967.8203 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2589 reflections read from tmp file 464 reflections are rejected (463 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 5 0 2 5 4 7 1 80 Initial Chi^2= 0.36886 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.34488 Current error model SIG(F2)^2 = 165.58*I_RAW + 0.00*I_BACK+(0.00241*)^2 Cycle 2, Chi^2= 1.80681 Current error model SIG(F2)^2 = 29.08*I_RAW + 0.00*I_BACK+(0.02864*)^2 Cycle 3, Chi^2= 0.98468 Current error model SIG(F2)^2 = 102.82*I_RAW + 0.00*I_BACK+(0.02192*)^2 Cycle 4, Chi^2= 1.00008 Current error model SIG(F2)^2 = 103.38*I_RAW + 0.00*I_BACK+(0.02133*)^2 Cycle 5, Chi^2= 0.99999 Current error model SIG(F2)^2 = 102.90*I_RAW + 0.00*I_BACK+(0.02143*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 102.90*I_RAW + 0.00*I_BACK+(0.02143*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5619658- 1211641 258 1923869.36 44.09 100.00 1204469- 663213 258 880328.79 38.33 100.00 658405- 283691 258 446146.19 36.64 100.00 283481- 170345 258 212335.92 32.99 100.00 170152- 135889 258 153153.40 26.94 100.00 135865- 95305 258 110871.85 21.36 100.00 95168- 74247 258 84826.85 18.17 100.00 74067- 5460 258 44201.19 13.27 100.00 5416- 3040 258 3971.35 4.98 98.84 3038- 859 267 2359.45 4.12 87.64 ------------------------------------------------------------------------------------ 5619658- 859 2589 384872.09 24.02 98.61 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 258 794147.82 36.69 99.61 1.39- 1.12 258 735979.16 30.10 100.00 1.12- 0.96 258 430731.00 27.77 100.00 0.96- 0.88 258 367899.99 24.62 100.00 0.88- 0.81 258 469415.87 28.08 99.61 0.81- 0.73 258 245195.15 19.78 99.61 0.73- 0.71 258 176022.86 17.78 93.80 0.71- 0.65 258 328080.13 23.93 99.22 0.65- 0.62 258 156579.63 15.70 96.12 0.62- 0.58 267 152766.01 16.00 98.13 ------------------------------------------------------------------------------------ 4.82- 0.58 2589 384872.09 24.02 98.61 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.39 258 794147.82 36.69 99.61 4.82- 1.12 516 765063.49 33.40 99.81 4.82- 0.96 774 653619.32 31.52 99.87 4.82- 0.88 1032 582189.49 29.80 99.90 4.82- 0.81 1290 559634.77 29.45 99.84 4.82- 0.73 1548 507228.16 27.84 99.81 4.82- 0.71 1806 459913.12 26.40 98.95 4.82- 0.65 2064 443434.00 26.10 98.98 4.82- 0.62 2322 411561.29 24.94 98.66 4.82- 0.58 2589 384872.09 24.02 98.61 ------------------------------------------------------------------------------------ 4.82- 0.58 2589 384872.09 24.02 98.61 Scale applied to data: s=0.177947 (maximum obs:5619657.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.040; Rsigma 0.027: data 2589 -> merged 110 With outlier rejection... Rint 0.038; Rsigma 0.027: data 2576 -> merged 110 Rejected total: 13, method kkm 12, method Blessing 1 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585937, 4.831758 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 14.70 100.00 147 1.61 - 1.21 10 10 23.40 100.00 234 1.17 - 1.01 10 10 30.30 100.00 303 0.99 - 0.89 10 10 30.10 100.00 301 0.88 - 0.81 10 10 29.20 100.00 292 0.81 - 0.74 10 10 24.40 100.00 244 0.73 - 0.71 10 10 27.70 100.00 277 0.70 - 0.66 10 10 23.50 100.00 235 0.66 - 0.64 10 10 21.00 100.00 210 0.63 - 0.60 10 10 20.60 100.00 206 --------------------------------------------------------------- 5.92 - 0.60 100 100 24.49 100.00 2449 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:11:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918875 5.916661 5.915847 60.0398 90.0760 60.0215 2403 Reflections read from file xs1714a.hkl; mean (I/sigma) = 30.65 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1180 1279 1191 1216 1825 1608 1595 2403 N (int>3sigma) = 0 1063 1279 1074 1134 1708 1471 1438 2179 Mean intensity = 0.0 55.7 26.5 55.1 59.8 45.3 63.4 61.0 61.6 Mean int/sigma = 0.0 30.5 26.1 29.9 30.3 28.8 31.3 30.6 30.6 Lattice type: P chosen Volume: 146.53 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.916 5.917 119.96 90.05 119.95 Niggli form: a.a = 34.987 b.b = 34.997 c.c = 35.007 b.c = -17.480 a.c = -0.028 a.b = -17.471 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.058 CUBIC F-lattice R(int) = 0.209 [ 2249] Vol = 586.1 Cell: 8.363 8.374 8.370 90.00 89.98 90.03 Volume: 586.13 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.057 RHOMBOHEDRAL R-lattice R(int) = 0.199 [ 1972] Vol = 439.6 Cell: 5.916 5.915 14.499 89.97 90.06 119.95 Volume: 439.60 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.057 RHOMBOHEDRAL R-lattice R(int) = 0.187 [ 626] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.499 89.97 90.06 119.95 Volume: 439.60 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.063 TETRAGONAL I-lattice R(int) = 0.171 [ 2006] Vol = 293.1 Cell: 5.920 5.920 8.363 89.97 90.01 90.03 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.050 TETRAGONAL I-lattice R(int) = 0.171 [ 2006] Vol = 293.1 Cell: 5.920 5.920 8.363 89.97 90.01 90.03 Volume: 293.06 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.028 ORTHORHOMBIC I-lattice R(int) = 0.171 [ 1957] Vol = 293.1 Cell: 5.920 8.363 5.920 89.97 89.97 89.99 Volume: 293.06 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.015 MONOCLINIC I-lattice R(int) = 0.160 [ 1629] Vol = 293.1 Cell: 8.363 5.920 5.920 90.03 90.03 89.99 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.036 MONOCLINIC I-lattice R(int) = 0.161 [ 1636] Vol = 293.1 Cell: 5.917 5.915 8.374 89.98 90.02 89.95 Volume: 293.06 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.038 MONOCLINIC C-lattice R(int) = 0.143 [ 1653] Vol = 293.1 Cell: 8.363 8.374 5.915 89.98 134.97 90.03 Volume: 293.06 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.124 [ 1096] Vol = 146.5 Cell: 5.915 5.916 5.917 119.96 90.05 119.95 Volume: 146.53 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1279 0 1610 1608 2403 N (int>3sigma) = 0 0 0 0 1279 0 1459 1471 2179 Mean intensity = 0.0 0.0 0.0 0.0 26.5 0.0 62.2 63.4 61.6 Mean int/sigma = 0.0 0.0 0.0 0.0 26.1 0.0 31.0 31.3 30.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.165 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 22 22 170 563 N I>3s 19 19 119 563 0.7 0.7 0.6 31.9 6.4 6.4 3.9 32.3 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.209 2098 Fd-3m 1 1 227 C N N N N 37 2284 0.210 2136 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362860 8.373961 8.369626 90.0012 89.9839 90.0293 ZERR 1.00 0.000297 0.001700 0.003751 0.0020 0.0125 0.0015 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4535074- 563967 574 571 27 21.1 1315141.48 40.36 0.035 0.041 560023- 132131 767 764 27 28.3 234440.54 31.57 0.043 0.057 115668- 38994 642 642 27 23.8 84953.85 18.22 0.054 0.069 11246- 1940 606 599 29 20.7 3773.94 4.94 0.148 0.190 ------------------------------------------------------------------------------------------- 4535074- 1940 2589 2576 110 23.4 383097.56 24.00 0.038 0.045 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 639 630 27 23.3 691050.33 33.21 0.036 0.041 0.023 1.01-0.78 796 795 28 28.4 360366.27 23.39 0.029 0.036 0.027 0.76-0.65 694 692 28 24.7 266761.24 20.63 0.046 0.055 0.032 0.65-0.59 460 459 27 17.0 175180.09 17.49 0.061 0.067 0.039 ------------------------------------------------------------------------------------------------------ inf-0.59 2589 2576 110 23.4 383097.56 24.00 0.038 0.045 0.027 inf-0.60 2460 2447 99 24.7 397045.00 24.48 0.037 0.044 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 630 27 27 100.0 23.3 691050.33 183.76 0.036 0.007 1.01-0.78 795 28 28 100.0 28.4 360366.27 134.35 0.029 0.005 0.76-0.65 692 28 28 100.0 24.7 266761.24 109.94 0.046 0.008 0.65-0.59 459 27 27 100.0 17.0 175180.09 84.73 0.061 0.013 -------------------------------------------------------------------------------------------- inf-0.59 2576 110 110 100.0 23.4 383097.56 131.03 0.038 0.007 inf-0.60 2447 99 99 100.0 24.7 397045.00 134.42 0.037 0.007 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:17:50 2018) ID: 2932; threads 39; handles 878; mem 519396.00 (1237700.00)kB; time: 1w 5d 0h 23m 20s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.2,peak PF: 697.1, WS: 298.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.0,peak PF: 697.1, WS: 299.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:17:50 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000013 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) 5.91502 ( 0.00079 ) 5.91640 ( 0.00079 ) 5.92265 ( 0.00063 ) 60.05206 ( 0.01245 ) 89.98756 ( 0.00964 ) 60.01743 ( 0.01389 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:17:50 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000013 0.000015 0.000014 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021547 -0.014368 0.007205 ( 0.000003 0.000002 0.000002 ) -0.014368 0.028728 -0.014368 ( 0.000002 0.000004 0.000002 ) 0.007205 -0.014368 0.021561 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(12) 89.988(10) 60.017(14) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.088 ( 0.105) | 1.078 ( 0.132) | 1.164 ( 0.408) | 0.84- 0.81 | 44 | 1.100 ( 0.103) | 1.018 ( 0.125) | 1.350 ( 0.509) | 0.81- 0.73 | 44 | 1.102 ( 0.084) | 0.995 ( 0.125) | 1.348 ( 0.505) | 0.73- 0.69 | 44 | 1.087 ( 0.077) | 0.931 ( 0.109) | 1.374 ( 0.487) | 0.69- 0.66 | 44 | 1.078 ( 0.073) | 0.883 ( 0.089) | 1.403 ( 0.484) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.062 ( 0.110) | 0.998 ( 0.252) | 1.319 ( 0.892) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070032 0.030484 0.088660 ( 0.000027 0.000026 0.000015 ) -0.068375 -0.065763 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109065 -0.152749 0.115659 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028586 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9266(15) 5.9308(15) 5.9443(11) 60.01(2) 90.018(18) 60.02(3) V = 147.79(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070137 0.030664 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109139 -0.153002 0.116012 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9214(14) 5.9313(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070137 0.030664 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109139 -0.153002 0.116012 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9214(14) 5.9313(10) 60.04(2) 90.042(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.708) | 1.567 ( 2.299) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.170 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.142) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.029 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.993 ( 0.128) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.063 ( 0.108) | 1.003 ( 0.281) | 1.324 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 484 peaks identified as outliers and rejected 474 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 474 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 474 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.032 ( 0.144) | 1.122 ( 0.424) | 1.109 ( 0.575) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.275 ( 0.643) | 1.092 ( 0.634) | 1.12- 0.98 | 47 | 1.019 ( 0.102) | 1.057 ( 0.160) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.029 ( 0.093) | 1.035 ( 0.135) | 1.097 ( 0.433) | 0.89- 0.82 | 47 | 1.036 ( 0.085) | 1.007 ( 0.124) | 1.151 ( 0.478) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.196 ( 0.514) | 0.75- 0.71 | 47 | 1.027 ( 0.045) | 0.938 ( 0.113) | 1.296 ( 0.513) | 0.71- 0.67 | 47 | 1.001 ( 0.040) | 0.889 ( 0.071) | 1.260 ( 0.499) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.301 ( 0.513) | 0.63- 0.59 | 51 | 0.945 ( 0.054) | 0.815 ( 0.041) | 1.344 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 474 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.182 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088653 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010206 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116127 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.014 ( 0.108) | 1.028 ( 0.130) | 0.949 ( 0.328) | 0.97- 0.89 | 47 | 1.028 ( 0.089) | 1.029 ( 0.137) | 1.105 ( 0.406) | 0.88- 0.82 | 47 | 1.047 ( 0.079) | 1.022 ( 0.118) | 1.207 ( 0.509) | 0.82- 0.75 | 47 | 1.037 ( 0.080) | 0.987 ( 0.126) | 1.069 ( 0.407) | 0.75- 0.71 | 47 | 1.022 ( 0.044) | 0.934 ( 0.110) | 1.339 ( 0.543) | 0.71- 0.67 | 47 | 0.997 ( 0.043) | 0.885 ( 0.072) | 1.211 ( 0.465) | 0.67- 0.63 | 47 | 0.974 ( 0.047) | 0.841 ( 0.041) | 1.288 ( 0.498) | 0.63- 0.59 | 49 | 0.949 ( 0.045) | 0.812 ( 0.041) | 1.347 ( 0.519) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 472 | 1.014 ( 0.090) | 0.993 ( 0.294) | 1.173 ( 0.533) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb PROFFITPEAK info: 569 peaks in the peak location table UB fit with 254 obs out of 271 (total:271,skipped:0) (93.73%) UB - matrix: -0.069441 0.031065 0.089172 ( 0.000065 0.000103 0.000145 ) -0.069072 -0.065344 -0.010282 ( 0.000052 0.000081 0.000115 ) 0.109036 -0.153186 0.116374 ( 0.000079 0.000124 0.000175 ) M - matrix: 0.021482 -0.014346 0.007207 ( 0.000021 0.000021 0.000025 ) -0.014346 0.028701 -0.014385 ( 0.000021 0.000040 0.000033 ) 0.007207 -0.014385 0.021600 ( 0.000025 0.000033 0.000048 ) unit cell: 5.929(5) 5.922(5) 5.913(6) 60.01(10) 90.07(8) 60.01(9) V = 146.8(2) UB fit with 254 obs out of 271 (total:271,skipped:0) (93.73%) UB - matrix: -0.069441 0.031065 0.089172 ( 0.000065 0.000103 0.000145 ) -0.069072 -0.065344 -0.010282 ( 0.000052 0.000081 0.000115 ) 0.109036 -0.153186 0.116374 ( 0.000079 0.000124 0.000175 ) M - matrix: 0.021482 -0.014346 0.007207 ( 0.000021 0.000021 0.000025 ) -0.014346 0.028701 -0.014385 ( 0.000021 0.000040 0.000033 ) 0.007207 -0.014385 0.021600 ( 0.000025 0.000033 0.000048 ) unit cell: 5.929(5) 5.922(5) 5.913(6) 60.01(10) 90.07(8) 60.01(9) V = 146.8(2) OTKP changes: 50 1 1 1 UB - matrix: -0.069532 0.031266 0.089052 ( 0.000068 0.000108 0.000150 ) -0.068753 -0.065496 -0.010069 ( 0.000054 0.000086 0.000120 ) 0.109231 -0.153280 0.116543 ( 0.000079 0.000125 0.000174 ) M - matrix: 0.021493 -0.014414 0.007230 ( 0.000021 0.000021 0.000026 ) -0.014414 0.028762 -0.014420 ( 0.000021 0.000041 0.000033 ) 0.007230 -0.014420 0.021614 ( 0.000026 0.000033 0.000049 ) UB fit with 259 obs out of 271 (total:271,skipped:0) (95.57%) unit cell: 5.938(5) 5.927(5) 5.914(6) 59.99(10) 90.02(8) 59.88(9) V = 146.9(2) UB fit with 259 obs out of 271 (total:271,skipped:0) (95.57%) UB - matrix: -0.069532 0.031266 0.089052 ( 0.000068 0.000108 0.000150 ) -0.068753 -0.065496 -0.010069 ( 0.000054 0.000086 0.000120 ) 0.109231 -0.153280 0.116543 ( 0.000079 0.000125 0.000174 ) M - matrix: 0.021493 -0.014414 0.007230 ( 0.000021 0.000021 0.000026 ) -0.014414 0.028762 -0.014420 ( 0.000021 0.000041 0.000033 ) 0.007230 -0.014420 0.021614 ( 0.000026 0.000033 0.000049 ) unit cell: 5.938(5) 5.927(5) 5.914(6) 59.99(10) 90.02(8) 59.88(9) V = 146.9(2) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 271 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Run 5 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.997) HKL list info: 430 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069532 0.031266 0.089052 ( 0.000068 0.000108 0.000150 ) -0.068753 -0.065496 -0.010069 ( 0.000054 0.000086 0.000120 ) 0.109231 -0.153280 0.116543 ( 0.000079 0.000125 0.000174 ) M - matrix: 0.021493 -0.014414 0.007230 ( 0.000021 0.000021 0.000026 ) -0.014414 0.028762 -0.014420 ( 0.000021 0.000041 0.000033 ) 0.007230 -0.014420 0.021614 ( 0.000026 0.000033 0.000049 ) UB fit with 259 obs out of 271 (total:271,skipped:0) (95.57%) unit cell: 5.938(5) 5.927(5) 5.914(6) 59.99(10) 90.02(8) 59.88(9) V = 146.9(2) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 259 obs out of 271 (total:271,skipped:0) (95.57%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb 2 of 221 peaks identified as outliers and rejected 219 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 219 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 219 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.61 | 22 | 1.030 ( 0.244) | 1.321 ( 0.748) | 1.280 ( 0.833) | 1.60- 1.17 | 22 | 1.013 ( 0.093) | 1.035 ( 0.130) | 0.850 ( 0.310) | 1.17- 0.98 | 22 | 1.015 ( 0.078) | 1.017 ( 0.124) | 1.090 ( 0.478) | 0.97- 0.92 | 22 | 1.005 ( 0.077) | 1.001 ( 0.131) | 1.119 ( 0.431) | 0.89- 0.82 | 22 | 1.007 ( 0.070) | 0.970 ( 0.108) | 1.140 ( 0.513) | 0.82- 0.76 | 22 | 1.020 ( 0.079) | 0.988 ( 0.119) | 1.201 ( 0.426) | 0.76- 0.71 | 22 | 0.980 ( 0.053) | 0.926 ( 0.068) | 1.352 ( 0.449) | 0.71- 0.67 | 22 | 0.960 ( 0.042) | 0.874 ( 0.050) | 1.301 ( 0.529) | 0.67- 0.63 | 22 | 0.932 ( 0.041) | 0.836 ( 0.032) | 1.406 ( 0.463) | 0.63- 0.59 | 21 | 0.901 ( 0.033) | 0.811 ( 0.031) | 1.493 ( 0.620) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 219 | 0.987 ( 0.107) | 0.979 ( 0.288) | 1.222 ( 0.550) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) UB - matrix: -0.069804 0.031296 0.088955 ( 0.000029 0.000048 0.000064 ) -0.068888 -0.065428 -0.010204 ( 0.000025 0.000042 0.000056 ) 0.109238 -0.152975 0.116290 ( 0.000032 0.000054 0.000072 ) M - matrix: 0.021551 -0.014388 0.007197 ( 0.000009 0.000009 0.000011 ) -0.014388 0.028662 -0.014338 ( 0.000009 0.000018 0.000014 ) 0.007197 -0.014338 0.021541 ( 0.000011 0.000014 0.000020 ) unit cell: 5.926(2) 5.930(2) 5.917(3) 60.05(5) 90.00(4) 59.89(4) V = 146.91(10) OTKP changes: 219 1 1 1 UB - matrix: -0.069744 0.031280 0.089067 ( 0.000026 0.000044 0.000059 ) -0.069061 -0.065470 -0.010301 ( 0.000025 0.000042 0.000055 ) 0.109118 -0.153263 0.116365 ( 0.000027 0.000045 0.000060 ) M - matrix: 0.021540 -0.014384 0.007197 ( 0.000008 0.000008 0.000009 ) -0.014384 0.028754 -0.014374 ( 0.000008 0.000015 0.000012 ) 0.007197 -0.014374 0.021580 ( 0.000009 0.000012 0.000017 ) UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) unit cell: 5.922(2) 5.916(2) 5.912(2) 60.04(4) 90.03(3) 59.97(4) V = 146.45(9) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.847) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069744 0.031280 0.089067 ( 0.000026 0.000044 0.000059 ) -0.069061 -0.065470 -0.010301 ( 0.000025 0.000042 0.000055 ) 0.109118 -0.153263 0.116365 ( 0.000027 0.000045 0.000060 ) M - matrix: 0.021540 -0.014384 0.007197 ( 0.000008 0.000008 0.000009 ) -0.014384 0.028754 -0.014374 ( 0.000008 0.000015 0.000012 ) 0.007197 -0.014374 0.021580 ( 0.000009 0.000012 0.000017 ) UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) unit cell: 5.922(2) 5.916(2) 5.912(2) 60.04(4) 90.03(3) 59.97(4) V = 146.45(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 219 obs out of 219 (total:219,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb 2 of 224 peaks identified as outliers and rejected 222 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 222 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 222 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.61 | 22 | 1.053 ( 0.245) | 1.234 ( 0.723) | 1.318 ( 0.954) | 1.61- 1.17 | 22 | 1.000 ( 0.109) | 1.021 ( 0.150) | 0.864 ( 0.315) | 1.17- 1.02 | 22 | 1.003 ( 0.084) | 1.024 ( 0.136) | 1.055 ( 0.396) | 0.99- 0.92 | 22 | 1.011 ( 0.081) | 1.022 ( 0.124) | 1.011 ( 0.424) | 0.92- 0.84 | 22 | 1.012 ( 0.074) | 0.978 ( 0.096) | 1.146 ( 0.420) | 0.84- 0.78 | 22 | 1.013 ( 0.087) | 0.971 ( 0.127) | 1.215 ( 0.503) | 0.76- 0.72 | 22 | 0.988 ( 0.056) | 0.930 ( 0.073) | 1.464 ( 0.443) | 0.71- 0.67 | 22 | 0.974 ( 0.039) | 0.896 ( 0.065) | 1.445 ( 0.586) | 0.67- 0.64 | 22 | 0.929 ( 0.039) | 0.841 ( 0.033) | 1.308 ( 0.505) | 0.64- 0.59 | 24 | 0.907 ( 0.037) | 0.815 ( 0.031) | 1.480 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 222 | 0.988 ( 0.111) | 0.972 ( 0.272) | 1.233 ( 0.575) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 202 | 1.121 ( 0.130) | 1.230 ( 0.439) | 1.231 ( 1.187) | 13.3-19.0 | 202 | 1.081 ( 0.055) | 1.135 ( 0.287) | 1.195 ( 0.521) | 19.0-23.1 | 202 | 1.070 ( 0.072) | 1.151 ( 0.404) | 1.196 ( 0.538) | 23.1-27.2 | 203 | 1.035 ( 0.077) | 1.070 ( 0.267) | 1.193 ( 0.572) | 27.2-30.8 | 202 | 1.012 ( 0.073) | 1.010 ( 0.247) | 1.191 ( 0.506) | 30.8-33.8 | 202 | 0.983 ( 0.081) | 0.921 ( 0.105) | 1.207 ( 0.511) | 33.8-36.9 | 202 | 0.963 ( 0.075) | 0.900 ( 0.094) | 1.177 ( 0.483) | 36.9-39.6 | 202 | 0.950 ( 0.087) | 0.872 ( 0.136) | 1.210 ( 0.555) | 39.6-42.7 | 202 | 0.927 ( 0.075) | 0.836 ( 0.079) | 1.218 ( 0.527) | 42.7-49.9 | 202 | 0.932 ( 0.087) | 0.811 ( 0.066) | 1.144 ( 0.476) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2021 | 1.007 ( 0.105) | 0.994 ( 0.285) | 1.196 ( 0.621) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0097 b=1.26 e3 dimension: a=0.0025 b=1.00 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706998 Maximum peak integral for reflections I/sig<= 10000 - raw: 10471127 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:18:11 2018 PROFFITMAIN - Started at Tue Mar 27 15:18:11 2018 OTKP changes: 2021 2 4 5 OTKP changes: 2021 2 4 5 UB - matrix: -0.070109 0.031142 0.088927 ( 0.000011 0.000013 0.000012 ) -0.068745 -0.065911 -0.010401 ( 0.000011 0.000013 0.000012 ) 0.109155 -0.153031 0.116332 ( 0.000009 0.000011 0.000010 ) M - matrix: 0.021556 -0.014356 0.007179 ( 0.000003 0.000002 0.000002 ) -0.014356 0.028733 -0.014347 ( 0.000002 0.000004 0.000002 ) 0.007179 -0.014347 0.021549 ( 0.000002 0.000002 0.000003 ) UB fit with 2021 obs out of 2021 (total:2021,skipped:0) (100.00%) unit cell: 5.9144(7) 5.9120(7) 5.9139(6) 60.055(11) 90.039(9) 60.032(12) V = 146.36(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070047 0.030661 0.088963 ( 0.000028 0.000028 0.000016 ) -0.068248 -0.066136 -0.010502 ( 0.000025 0.000025 0.000014 ) 0.109069 -0.153052 0.115967 ( 0.000025 0.000025 0.000014 ) M - matrix: 0.021460 -0.014327 0.007134 ( 0.000008 0.000006 0.000004 ) -0.014327 0.028739 -0.014327 ( 0.000006 0.000008 0.000004 ) 0.007134 -0.014327 0.021473 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9278(14) 5.9139(14) 5.9250(11) 60.02(2) 89.965(18) 60.00(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070349 0.030950 0.088809 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066148 -0.010664 ( 0.000024 0.000023 0.000013 ) 0.109348 -0.153293 0.116375 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014415 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028832 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014385 0.021544 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9071(13) 5.9177(10) 60.05(2) 90.061(16) 59.99(2) V = 146.22(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.784) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070349 0.030950 0.088809 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066148 -0.010664 ( 0.000024 0.000023 0.000013 ) 0.109348 -0.153293 0.116375 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014415 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028832 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014385 0.021544 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9071(13) 5.9177(10) 60.05(2) 90.061(16) 59.99(2) V = 146.22(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070349 0.030950 0.088809 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066148 -0.010664 ( 0.000024 0.000023 0.000013 ) 0.109348 -0.153293 0.116375 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021585 -0.014415 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014415 0.028832 -0.014385 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014385 0.021544 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9071(13) 5.9177(10) 60.05(2) 90.061(16) 59.99(2) V = 146.22(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070407 0.031349 0.088638 ( 0.000026 0.000022 0.000027 ) -0.068574 -0.066003 -0.010232 ( 0.000031 0.000027 0.000033 ) 0.108988 -0.152638 0.116246 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021538 -0.014317 0.007130 ( 0.000007 0.000005 0.000005 ) -0.014317 0.028638 -0.014289 ( 0.000005 0.000007 0.000005 ) 0.007130 -0.014289 0.021474 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(16) 5.9212(16) 5.9223(13) 60.03(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070369 0.031228 0.088844 ( 0.000023 0.000020 0.000025 ) -0.068806 -0.065847 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153155 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014386 0.007190 ( 0.000007 0.000005 0.000005 ) -0.014386 0.028768 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007190 -0.014400 0.021595 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9090(16) 5.9158(16) 5.9136(12) 59.95(2) 89.954(19) 60.01(3) V = 146.13(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.784) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070369 0.031228 0.088844 ( 0.000023 0.000020 0.000025 ) -0.068806 -0.065847 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153155 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014386 0.007190 ( 0.000007 0.000005 0.000005 ) -0.014386 0.028768 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007190 -0.014400 0.021595 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9090(16) 5.9158(16) 5.9136(12) 59.95(2) 89.954(19) 60.01(3) V = 146.13(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070369 0.031228 0.088844 ( 0.000023 0.000020 0.000025 ) -0.068806 -0.065847 -0.010366 ( 0.000030 0.000026 0.000032 ) 0.109168 -0.153155 0.116593 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021604 -0.014386 0.007190 ( 0.000007 0.000005 0.000005 ) -0.014386 0.028768 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007190 -0.014400 0.021595 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9090(16) 5.9158(16) 5.9136(12) 59.95(2) 89.954(19) 60.01(3) V = 146.13(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) UB - matrix: -0.070161 0.031462 0.088647 ( 0.000016 0.000026 0.000022 ) -0.068856 -0.065709 -0.010191 ( 0.000021 0.000032 0.000027 ) 0.108921 -0.152882 0.116149 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021527 -0.014335 0.007133 ( 0.000005 0.000005 0.000004 ) -0.014335 0.028680 -0.014299 ( 0.000005 0.000009 0.000005 ) 0.007133 -0.014299 0.021453 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9185(15) 5.9193(15) 5.9264(11) 60.03(2) 89.947(18) 59.99(3) V = 146.91(5) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 UB - matrix: -0.070150 0.031455 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068734 -0.066027 -0.009951 ( 0.000018 0.000028 0.000024 ) 0.109188 -0.153132 0.116582 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021567 -0.014388 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014388 0.028798 -0.014399 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014399 0.021591 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9131(14) 5.9126(11) 59.96(2) 89.934(17) 59.97(2) V = 146.18(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.784) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070150 0.031455 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068734 -0.066027 -0.009951 ( 0.000018 0.000028 0.000024 ) 0.109188 -0.153132 0.116582 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021567 -0.014388 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014388 0.028798 -0.014399 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014399 0.021591 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9131(14) 5.9126(11) 59.96(2) 89.934(17) 59.97(2) V = 146.18(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070150 0.031455 0.088888 ( 0.000016 0.000025 0.000021 ) -0.068734 -0.066027 -0.009951 ( 0.000018 0.000028 0.000024 ) 0.109188 -0.153132 0.116582 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021567 -0.014388 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014388 0.028798 -0.014399 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014399 0.021591 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9153(13) 5.9131(14) 5.9126(11) 59.96(2) 89.934(17) 59.97(2) V = 146.18(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) UB - matrix: -0.069966 0.031424 0.089010 ( 0.000026 0.000043 0.000058 ) -0.068955 -0.065540 -0.010302 ( 0.000028 0.000047 0.000063 ) 0.109256 -0.153158 0.116461 ( 0.000027 0.000045 0.000061 ) M - matrix: 0.021587 -0.014413 0.007207 ( 0.000008 0.000008 0.000010 ) -0.014413 0.028740 -0.014365 ( 0.000008 0.000015 0.000012 ) 0.007207 -0.014365 0.021592 ( 0.000010 0.000012 0.000018 ) unit cell: 5.919(3) 5.919(2) 5.908(3) 60.08(4) 90.01(3) 59.91(4) V = 146.32(10) OTKP changes: 222 1 1 1 UB - matrix: -0.069788 0.031286 0.089079 ( 0.000025 0.000041 0.000056 ) -0.069077 -0.065461 -0.010349 ( 0.000028 0.000047 0.000064 ) 0.109144 -0.153266 0.116392 ( 0.000024 0.000040 0.000054 ) M - matrix: 0.021555 -0.014390 0.007202 ( 0.000007 0.000007 0.000009 ) -0.014390 0.028754 -0.014375 ( 0.000007 0.000014 0.000011 ) 0.007202 -0.014375 0.021589 ( 0.000009 0.000011 0.000016 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 5.920(2) 5.916(2) 5.910(2) 60.06(4) 90.03(3) 59.96(4) V = 146.36(9) Run 5 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.834) HKL list info: 424 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069788 0.031286 0.089079 ( 0.000025 0.000041 0.000056 ) -0.069077 -0.065461 -0.010349 ( 0.000028 0.000047 0.000064 ) 0.109144 -0.153266 0.116392 ( 0.000024 0.000040 0.000054 ) M - matrix: 0.021555 -0.014390 0.007202 ( 0.000007 0.000007 0.000009 ) -0.014390 0.028754 -0.014375 ( 0.000007 0.000014 0.000011 ) 0.007202 -0.014375 0.021589 ( 0.000009 0.000011 0.000016 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 5.920(2) 5.916(2) 5.910(2) 60.06(4) 90.03(3) 59.96(4) V = 146.36(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.069788 0.031286 0.089079 ( 0.000025 0.000041 0.000056 ) -0.069077 -0.065461 -0.010349 ( 0.000028 0.000047 0.000064 ) 0.109144 -0.153266 0.116392 ( 0.000024 0.000040 0.000054 ) M - matrix: 0.021555 -0.014390 0.007202 ( 0.000007 0.000007 0.000009 ) -0.014390 0.028754 -0.014375 ( 0.000007 0.000014 0.000011 ) 0.007202 -0.014375 0.021589 ( 0.000009 0.000011 0.000016 ) UB fit with 222 obs out of 222 (total:222,skipped:0) (100.00%) unit cell: 5.920(2) 5.916(2) 5.910(2) 60.06(4) 90.03(3) 59.96(4) V = 146.36(9) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.069984 0.031117 0.088886 ( 0.000012 0.000013 0.000013 ) -0.068758 -0.065792 -0.010448 ( 0.000012 0.000014 0.000013 ) 0.109173 -0.153082 0.116424 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021544 -0.014366 0.007208 ( 0.000003 0.000002 0.000002 ) -0.014366 0.028731 -0.014369 ( 0.000002 0.000004 0.000002 ) 0.007208 -0.014369 0.021565 ( 0.000002 0.000002 0.000003 ) UB fit with 2021 obs out of 2021 (total:2021,skipped:0) (100.00%) unit cell: 5.9190(8) 5.9156(8) 5.9153(6) 60.046(12) 90.092(9) 60.033(14) V = 146.51(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 63 reflections under beam stop or inside a detector rejection region 17 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof 2744 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:18:16 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.784) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.784) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.784) Run 5 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.834) PROFFIT INFO: signal sum: min=235.0000 max=20922698.0000 PROFFIT INFO: signal sum lp corr: min=467.8904 max=2973725.9492 PROFFIT INFO: background sum: min=615.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=748.6246 max=4757961.5000 PROFFIT INFO: sig(Inet): min=122.9918 max=47812.0586 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=248.94 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 27 124 279 561 631 1103 1828 2511 2744 Percent 0.0 0.0 1.0 4.5 10.2 20.4 23.0 40.2 66.6 91.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2744 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2744 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4757962- 1181038 274 1910186.89 121.19 100.00 1178763- 658536 274 889090.25 105.05 100.00 656723- 273622 274 431287.38 96.11 100.00 273498- 174326 274 209075.35 71.50 100.00 174321- 125292 274 150775.81 51.98 100.00 124986- 97286 274 109938.44 36.70 100.00 97257- 70310 274 85147.80 30.02 100.00 70295- 5730 274 39141.86 19.37 100.00 5729- 3082 274 4072.80 5.28 97.08 3054- 749 278 2219.00 3.89 58.27 ------------------------------------------------------------------------------------ 4757962- 749 2744 382538.35 54.04 95.48 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 274 702066.51 87.46 98.91 1.32- 1.05 274 552696.47 67.18 97.81 1.05- 0.92 274 479312.13 62.91 98.18 0.92- 0.82 274 339038.47 52.25 95.62 0.82- 0.74 274 435966.38 58.62 95.99 0.74- 0.67 274 380444.38 57.27 96.72 0.67- 0.61 274 209293.80 38.28 94.16 0.61- 0.56 274 308378.47 46.19 91.97 0.56- 0.51 274 228223.30 38.21 91.24 0.51- 0.40 278 192734.42 32.31 94.24 ------------------------------------------------------------------------------------ 5.26- 0.40 2744 382538.35 54.04 95.48 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:18:16 2018 Sorting 2744 observations 294 unique observations with > 7.00 F2/sig(F2) 2744 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 49 470 Total number of frames 470 Maximum number of 294 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2744 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 24 238 Total number of frames 238 2207 observations > 7.00 F2/sig(F2) 2207 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 24 238 Total number of frames 238 Removing 'redundancy=1' reflections Average redundancy: 7.8 (Out of 2207 removed 29 = 2178, unique = 278) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2178 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 24 238 Total number of frames 238 278 unique data precomputed (should be 278) 278 unique data with 2178 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 7.8 (Out of 2178 removed 0 = 2178, unique = 278) 278 unique data precomputed (should be 278) 278 unique data with 2178 observations RMS deviation of equivalent data = 0.72651 Rint = 0.69427 11 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.67674, wR= 3.88303 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68769, wR= 3.09586, Acormin=0.118, Acormax=1.848, Acor_av=0.822 F test: Probability=0.000, F= 0.966 Trying model 2 (ne=2, no=1)... Results: Rint= 0.79875, wR= 3.01838, Acormin=-0.470, Acormax=1.853, Acor_av=0.599 F test: Probability=0.000, F= 0.715 Trying model 3 (ne=4, no=0)... Results: Rint= 0.72730, wR= 2.77673, Acormin=-0.093, Acormax=2.130, Acor_av=0.704 F test: Probability=0.000, F= 0.859 Trying model 4 (ne=4, no=1)... Results: Rint= 0.83560, wR= 2.70055, Acormin=-0.461, Acormax=1.913, Acor_av=0.504 F test: Probability=0.000, F= 0.650 Trying model 5 (ne=4, no=3)... Results: Rint= 0.88153, wR= 2.62504, Acormin=-1.240, Acormax=1.854, Acor_av=0.341 F test: Probability=0.000, F= 0.582 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75578, wR= 2.73971, Acormin=-0.363, Acormax=2.606, Acor_av=0.628 F test: Probability=0.000, F= 0.790 Trying model 7 (ne=6, no=1)... Results: Rint= 0.84381, wR= 2.75308, Acormin=-0.781, Acormax=2.036, Acor_av=0.436 F test: Probability=0.000, F= 0.633 Trying model 8 (ne=6, no=3)... Results: Rint= 0.88469, wR= 2.61023, Acormin=-1.338, Acormax=1.904, Acor_av=0.293 F test: Probability=0.000, F= 0.574 Trying model 9 (ne=6, no=5)... Results: Rint= 0.89263, wR= 2.67262, Acormin=-1.368, Acormax=2.089, Acor_av=0.253 F test: Probability=0.000, F= 0.560 Trying model 10 (ne=8, no=0)... Results: Rint= 0.84930, wR= 2.41897, Acormin=-0.684, Acormax=2.103, Acor_av=0.420 F test: Probability=0.000, F= 0.620 Trying model 11 (ne=8, no=1)... Results: Rint= 0.93231, wR= 2.09086, Acormin=-1.168, Acormax=1.472, Acor_av=0.177 F test: Probability=0.000, F= 0.514 Trying model 12 (ne=8, no=3)... Results: Rint= 0.99279, wR= 1.65470, Acormin=-0.046, Acormax=0.069, Acor_av=0.002 F test: Probability=0.000, F= 0.451 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99465, wR= 1.64687, Acormin=-0.046, Acormax=0.073, Acor_av=0.002 F test: Probability=0.000, F= 0.447 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00833, wR= 1.69928, Acormin=-0.042, Acormax=0.071, Acor_av=0.002 F test: Probability=0.000, F= 0.431 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86252 There are 238 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 242 pars with 29403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.72651 Using Levenberg-Marquardt: 0.00010 New wR= 0.70694 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.69427 with corrections 0.67448 Rint for all data: 0.86252 with corrections 0.84725 13 observations identified as outliers and rejected Cycle 2 wR= 0.68193 Using Levenberg-Marquardt: 0.00001 New wR= 0.67856 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67302 with corrections 0.65146 Rint for all data: 0.86252 with corrections 0.84811 11 observations identified as outliers and rejected Cycle 3 wR= 0.65787 Using Levenberg-Marquardt: 0.00000 New wR= 0.65840 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66113 with corrections 0.65056 Rint for all data: 0.86252 with corrections 0.85527 Final wR= 0.65840 Final frame scales: Min= 1.0000 Max= 5.7895 Final absorption correction factors: Amin= 0.4361 Amax= 1.5544 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 238 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 242 pars with 29403 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.85151 Using Levenberg-Marquardt: 0.00010 New wR= 0.73479 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66113 with corrections 1.46333 Rint for all data: 0.86252 with corrections 1.50120 8 observations identified as outliers and rejected Cycle 2 wR= 0.71828 Using Levenberg-Marquardt: 0.00001 New wR= 0.64557 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65779 with corrections 0.75206 Rint for all data: 0.86252 with corrections 0.92168 8 observations identified as outliers and rejected Cycle 3 wR= 0.63560 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 New wR= 0.69689 Using Levenberg-Marquardt: 0.01000 New wR= 0.62186 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65366 with corrections 0.68595 Rint for all data: 0.86252 with corrections 0.87975 4 observations identified as outliers and rejected Cycle 4 wR= 0.62047 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61861 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65169 with corrections 0.67043 Rint for all data: 0.86252 with corrections 0.87208 1 observations identified as outliers and rejected Cycle 5 wR= 0.61482 Using Levenberg-Marquardt: 0.01000 New wR= 0.61358 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65041 with corrections 0.66894 Rint for all data: 0.86252 with corrections 0.87191 0 observations identified as outliers and rejected Final wR= 0.61358 Final frame scales: Min= 1.0000 Max= 10.2888 Final absorption correction factors: Amin= 0.1775 Amax= 1.7386 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 116 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 120 pars with 7260 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.86675 Using Levenberg-Marquardt: 0.00010 New wR= 0.78776 There are 10 clusters with unrefined scales (size 1-50) Rint for refined data: 0.65041 with corrections 1.20389 Rint for all data: 0.86252 with corrections 1.28933 10 observations identified as outliers and rejected Cycle 2 wR= 0.71645 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.70592 There are 10 clusters with unrefined scales (size 1-50) Rint for refined data: 0.64812 with corrections 1.14116 Rint for all data: 0.86252 with corrections 1.26395 2 observations identified as outliers and rejected Cycle 3 wR= 0.70393 Using Levenberg-Marquardt: 1.00000 New wR= 0.66248 There are 10 clusters with unrefined scales (size 1-50) Rint for refined data: 0.64777 with corrections 0.97750 Rint for all data: 0.86252 with corrections 1.09881 1 observations identified as outliers and rejected Cycle 4 wR= 0.66144 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.63208 There are 10 clusters with unrefined scales (size 1-50) Rint for refined data: 0.64768 with corrections 0.81219 Rint for all data: 0.86252 with corrections 0.97408 2 observations identified as outliers and rejected Cycle 5 wR= 0.62378 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.60477 There are 10 clusters with unrefined scales (size 1-50) Rint for refined data: 0.64721 with corrections 0.68850 Rint for all data: 0.86252 with corrections 0.88425 0 observations identified as outliers and rejected Final wR= 0.60477 Final frame scales: Min= 0.7666 Max= 4.6029 Final absorption correction factors: Amin= 0.0069 Amax= 2.2423 PROFFIT INFO: Inet (after scale3 abspack): min=590.9652 max=8169304.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=104.0182 max=92584.8828 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2744 reflections read from tmp file 2294 reflections are rejected (2219 as outliers, 75 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7+ Number of groups: 0 96 41 12 10 5 1 Initial Chi^2= 1.26528 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.77639 Current error model SIG(F2)^2 = 428.06*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 332.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 332.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 8169304- 1029072 274 1673384.98 75.27 100.00 1026183- 580180 274 784117.89 43.78 100.00 579261- 214689 274 360061.49 34.20 100.00 214055- 150609 274 178213.15 25.90 100.00 150565- 115414 274 130062.09 20.44 100.00 115181- 85402 274 100852.87 15.62 100.00 85397- 61568 274 73103.40 12.65 100.00 61393- 5941 274 34694.02 8.09 81.75 5939- 2432 274 3718.57 2.81 17.52 2427- 591 278 1757.76 2.54 19.06 ------------------------------------------------------------------------------------ 8169304- 591 2744 333512.31 24.10 81.74 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 274 558136.57 54.02 94.53 1.32- 1.05 274 452821.14 34.70 88.69 1.05- 0.92 274 424461.53 29.37 86.50 0.92- 0.82 274 269372.47 21.28 77.37 0.82- 0.74 274 381888.20 23.56 82.85 0.74- 0.67 274 328673.75 21.10 81.39 0.67- 0.61 274 189139.10 14.14 76.28 0.61- 0.56 274 276528.74 16.92 78.10 0.56- 0.51 274 235107.77 14.07 78.10 0.51- 0.40 278 220641.55 12.01 73.74 ------------------------------------------------------------------------------------ 5.26- 0.40 2744 333512.31 24.10 81.74 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 274 558136.57 54.02 94.53 5.26- 1.05 548 505478.85 44.36 91.61 5.26- 0.92 822 478473.08 39.36 89.90 5.26- 0.82 1096 426197.93 34.84 86.77 5.26- 0.74 1370 417335.98 32.59 85.99 5.26- 0.67 1644 402558.94 30.67 85.22 5.26- 0.61 1918 372070.39 28.31 83.94 5.26- 0.56 2192 360127.69 26.89 83.21 5.26- 0.51 2466 346236.59 25.46 82.64 5.26- 0.40 2744 333512.31 24.10 81.74 ------------------------------------------------------------------------------------ 5.26- 0.40 2744 333512.31 24.10 81.74 Scale applied to data: s=0.122409 (maximum obs:8169304.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.884; Rsigma 0.029: data 2744 -> merged 316 With outlier rejection... Rint 0.815; Rsigma 0.029: data 2540 -> merged 316 Rejected total: 204, method kkm 188, method Blessing 16 Completeness direct cell (a, b, c) = (5.272, 5.272, 5.272), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404329, 5.271804 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 12.40 100.00 186 1.46 - 1.12 15 15 19.60 100.00 294 1.08 - 0.96 15 15 16.47 100.00 247 0.96 - 0.86 15 15 15.00 100.00 225 0.86 - 0.79 15 15 13.53 100.00 203 0.79 - 0.73 15 15 11.33 100.00 170 0.73 - 0.69 15 15 11.00 100.00 165 0.69 - 0.65 15 15 10.87 100.00 163 0.65 - 0.63 15 15 6.53 100.00 98 0.63 - 0.60 21 21 7.29 100.00 153 --------------------------------------------------------------- 5.92 - 0.60 156 156 12.21 100.00 1904 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:18:17 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918951 5.915618 5.915333 60.0462 90.0920 60.0327 2540 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1272 1359 1247 1282 1939 1697 1687 2540 N (int>3sigma) = 0 1009 1359 984 1025 1676 1391 1365 2061 Mean intensity = 0.0 33.4 16.1 33.7 35.7 27.5 38.2 37.4 37.2 Mean int/sigma = 0.0 22.7 19.9 22.4 22.9 21.6 24.2 23.6 23.6 Lattice type: P chosen Volume: 146.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.916 119.95 90.05 119.94 Niggli form: a.a = 34.984 b.b = 34.991 c.c = 34.995 b.c = -17.472 a.c = -0.033 a.b = -17.463 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.273 [ 2386] Vol = 586.1 Cell: 8.361 8.375 8.369 89.99 89.99 90.04 Volume: 586.05 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.268 [ 2109] Vol = 439.5 Cell: 5.915 5.915 14.498 89.97 90.07 119.94 Volume: 439.54 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.258 [ 673] Vol = 439.5 Trigonal Cell: 5.915 5.915 14.498 89.97 90.07 119.94 Volume: 439.54 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.071 TETRAGONAL I-lattice R(int) = 0.247 [ 2143] Vol = 293.0 Cell: 5.920 5.920 8.361 89.97 90.02 90.04 Volume: 293.03 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.247 [ 2143] Vol = 293.0 Cell: 5.920 5.920 8.361 89.97 90.02 90.04 Volume: 293.03 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.025 ORTHORHOMBIC I-lattice R(int) = 0.248 [ 2089] Vol = 293.0 Cell: 5.920 8.361 5.920 89.97 89.96 89.98 Volume: 293.03 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.243 [ 1764] Vol = 293.0 Cell: 8.361 5.920 5.920 90.04 90.03 89.98 Volume: 293.03 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.044 MONOCLINIC I-lattice R(int) = 0.241 [ 1766] Vol = 293.0 Cell: 5.916 5.915 8.375 89.97 90.02 89.95 Volume: 293.03 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.046 MONOCLINIC C-lattice R(int) = 0.229 [ 1792] Vol = 293.0 Cell: 8.361 8.375 5.915 89.97 134.97 90.04 Volume: 293.03 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.210 [ 1205] Vol = 146.5 Cell: 5.915 5.915 5.916 119.95 90.05 119.94 Volume: 146.51 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1359 0 1687 1697 2540 N (int>3sigma) = 0 0 0 0 1359 0 1382 1391 2061 Mean intensity = 0.0 0.0 0.0 0.0 16.1 0.0 36.8 38.2 37.2 Mean int/sigma = 0.0 0.0 0.0 0.0 19.9 0.0 23.6 24.2 23.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.173 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 186 601 N I>3s 20 20 65 601 0.4 0.4 0.4 17.6 5.7 5.7 3.2 24.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.273 2219 Fd-3m 1 1 227 C N N N N 37 2284 0.274 2257 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361382 8.374819 8.369208 89.9942 89.9911 90.0350 ZERR 1.00 0.000292 0.001681 0.003649 0.0017 0.0122 0.0013 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2216416- 619946 294 263 31 8.5 888326.19 50.08 0.645 0.636 617293- 478124 328 322 31 10.4 537307.55 33.44 0.907 0.915 477949- 384871 335 307 31 9.9 390556.25 30.15 1.014 1.033 380052- 279559 333 313 31 10.1 295261.16 25.12 0.996 1.080 277307- 217585 310 281 31 9.1 189874.16 20.13 0.856 1.025 215866- 162913 249 218 31 7.0 135659.21 14.28 0.714 0.725 162583- 110272 288 271 31 8.7 118963.77 16.90 0.569 0.547 110060- 87945 190 176 31 5.7 85075.07 11.04 0.502 0.397 86681- 57763 239 228 31 7.4 69654.68 11.35 0.622 0.579 56985- 1740 178 161 37 4.4 38330.16 6.54 0.691 0.631 ------------------------------------------------------------------------------------------- 2216416- 1740 2744 2540 316 8.0 303603.74 23.62 0.815 0.807 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 527 504 31 16.3 505160.48 44.98 0.847 0.953 0.016 1.05-0.83 490 471 31 15.2 329100.55 25.81 0.896 1.067 0.026 0.83-0.72 392 377 31 12.2 298752.09 21.34 0.836 0.953 0.030 0.72-0.65 363 343 34 10.1 238333.71 17.50 0.844 0.922 0.036 0.64-0.60 259 233 31 7.5 247320.05 15.98 0.768 0.843 0.039 0.59-0.56 229 204 35 5.8 152484.90 12.16 0.638 0.519 0.053 0.55-0.52 182 161 31 5.2 233607.26 14.32 0.731 0.785 0.044 0.51-0.49 140 114 32 3.6 133981.47 10.15 0.496 0.416 0.062 0.49-0.45 98 79 32 2.5 169658.37 10.69 0.418 0.383 0.058 0.45-0.40 64 54 28 1.9 224964.69 11.24 0.387 0.345 0.058 ------------------------------------------------------------------------------------------------------ inf-0.40 2744 2540 316 8.0 303603.74 23.62 0.815 0.807 0.029 inf-0.60 2006 1904 156 12.2 345504.33 27.42 0.851 0.958 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 504 31 31 100.0 16.3 505160.48 192.37 0.847 0.005 1.05-0.83 471 31 31 100.0 15.2 329100.55 113.87 0.896 0.010 0.83-0.72 377 31 31 100.0 12.2 298752.09 88.77 0.836 0.012 0.72-0.65 343 34 34 100.0 10.1 238333.71 67.29 0.844 0.017 0.64-0.60 233 31 31 100.0 7.5 247320.05 55.21 0.768 0.020 0.59-0.56 204 38 35 92.1 5.8 152484.90 37.54 0.638 0.031 0.55-0.52 161 37 31 83.8 5.2 233607.26 40.78 0.731 0.026 0.51-0.49 114 44 32 72.7 3.6 133981.47 22.77 0.496 0.041 0.49-0.45 79 61 32 52.5 2.5 169658.37 18.09 0.418 0.038 0.45-0.40 54 123 28 22.8 1.9 224964.69 16.70 0.387 0.041 -------------------------------------------------------------------------------------------- inf-0.40 2540 463 316 68.3 8.0 303603.74 94.15 0.815 0.019 inf-0.60 1904 156 156 100.0 12.2 345504.33 114.83 0.851 0.011 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 RRPPROF to HKL transformation matrix: -1.0 0.0 -1.0 1.0 0.0 -1.0 1.0 -2.0 1.0 No constraint UB - matrix: -0.025007 -0.079436 -0.015558 ( 0.000006 0.000007 0.000007 ) 0.072499 -0.029154 0.032896 ( 0.000007 0.000007 0.000007 ) -0.036257 -0.003626 0.076541 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007196 0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007173 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000001 0.007183 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025007 -0.079436 -0.015558 ( 0.000006 0.000007 0.000007 ) 0.072499 -0.029154 0.032896 ( 0.000007 0.000007 0.000007 ) -0.036257 -0.003626 0.076541 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3615(7) 8.3748(7) 8.3693(5) 89.994(6) 89.991(6) 90.034(6) V = 586.06(8) unit cell: 8.36852(19) 8.36852(19) 8.36852(19) 90.0 90.0 90.0 V = 586.06(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.784) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.784) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.784) Run 5 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.834) PROFFIT INFO: signal sum: min=235.0000 max=20922698.0000 PROFFIT INFO: signal sum lp corr: min=467.8904 max=2973725.9492 PROFFIT INFO: background sum: min=615.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=748.6246 max=4757961.5000 PROFFIT INFO: sig(Inet): min=122.9918 max=47812.0586 PROFFIT INFO: Inet/sig(Inet): min=1.02 max=248.94 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 0 54 248 558 1122 1262 2206 3656 5022 5488 Percent 0.0 0.0 1.0 4.5 10.2 20.4 23.0 40.2 66.6 91.5 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2744 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2744 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4757962- 1181038 274 1910186.89 121.19 100.00 1178763- 658536 274 889090.25 105.05 100.00 656723- 273622 274 431287.38 96.11 100.00 273498- 174326 274 209075.35 71.50 100.00 174321- 125292 274 150775.81 51.98 100.00 124986- 97286 274 109938.44 36.70 100.00 97257- 70310 274 85147.80 30.02 100.00 70295- 5730 274 39141.86 19.37 100.00 5729- 3082 274 4072.80 5.28 97.08 3054- 749 278 2219.00 3.89 58.27 ------------------------------------------------------------------------------------ 4757962- 749 2744 382538.35 54.04 95.48 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 274 752637.22 95.22 100.00 1.39- 1.12 274 690367.47 63.06 99.64 1.12- 0.96 274 454530.71 69.10 97.45 0.96- 0.88 274 375036.20 61.70 95.26 0.88- 0.81 274 468935.88 69.78 99.27 0.81- 0.73 274 250228.73 41.35 97.45 0.73- 0.71 274 182492.86 34.34 86.50 0.71- 0.65 274 331155.38 49.25 95.62 0.65- 0.62 274 163246.64 28.45 88.32 0.62- 0.58 278 160001.10 28.49 95.32 ------------------------------------------------------------------------------------ 4.82- 0.58 2744 382538.35 54.04 95.48 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:18:18 2018 Sorting 2744 observations 85 unique observations with > 7.00 F2/sig(F2) 2744 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 49 470 Total number of frames 470 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2744 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 8 81 Total number of frames 81 2207 observations > 7.00 F2/sig(F2) 2207 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 8 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 23.7 (Out of 2207 removed 3 = 2204, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2204 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 8 81 Total number of frames 81 93 unique data precomputed (should be 93) 93 unique data with 2204 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.7 (Out of 2204 removed 0 = 2204, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2204 observations RMS deviation of equivalent data = 0.23264 Rint = 0.15572 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.15064, wR= 0.23811 Trying model 1 (ne=2, no=0)... Results: Rint= 0.11666, wR= 0.15922, Acormin=0.667, Acormax=1.383, Acor_av=0.962 F test: Probability=1.000, F= 1.663 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11129, wR= 0.14279, Acormin=0.553, Acormax=1.464, Acor_av=0.867 F test: Probability=0.983, F= 1.097 Trying model 3 (ne=4, no=0)... Results: Rint= 0.09554, wR= 0.12998, Acormin=0.607, Acormax=1.497, Acor_av=0.926 F test: Probability=1.000, F= 1.353 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08503, wR= 0.11409, Acormin=0.485, Acormax=1.555, Acor_av=0.829 F test: Probability=1.000, F= 1.261 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07337, wR= 0.10339, Acormin=0.394, Acormax=1.583, Acor_av=0.816 F test: Probability=1.000, F= 1.339 Trying model 6 (ne=6, no=0)... Results: Rint= 0.08785, wR= 0.12277, Acormin=0.651, Acormax=1.550, Acor_av=0.933 F test: Probability=0.000, F= 0.697 Trying model 7 (ne=6, no=1)... Results: Rint= 0.07752, wR= 0.10766, Acormin=0.480, Acormax=1.582, Acor_av=0.837 F test: Probability=0.000, F= 0.893 Trying model 8 (ne=6, no=3)... Results: Rint= 0.06848, wR= 0.09834, Acormin=0.403, Acormax=1.589, Acor_av=0.829 F test: Probability=0.999, F= 1.141 Trying model 9 (ne=6, no=5)... Results: Rint= 0.06800, wR= 0.09396, Acormin=0.282, Acormax=1.337, Acor_av=0.709 F test: Probability=0.578, F= 1.009 Trying model 10 (ne=8, no=0)... Results: Rint= 0.08620, wR= 0.11754, Acormin=0.514, Acormax=1.496, Acor_av=0.840 F test: Probability=0.000, F= 0.629 Trying model 11 (ne=8, no=1)... Results: Rint= 0.07147, wR= 0.09908, Acormin=0.469, Acormax=1.625, Acor_av=0.854 F test: Probability=0.000, F= 0.914 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07115, wR= 0.09840, Acormin=0.155, Acormax=0.529, Acor_av=0.283 F test: Probability=0.000, F= 0.919 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06178, wR= 0.08748, Acormin=0.163, Acormax=0.613, Acor_av=0.326 F test: Probability=1.000, F= 1.212 Trying model 14 (ne=8, no=7)... Results: Rint= 0.05333, wR= 0.07728, Acormin=0.193, Acormax=0.717, Acor_av=0.358 F test: Probability=1.000, F= 1.614 Final absorption model (ne=6, no=3): Rint= 0.06848, Acormin=0.403, Acormax=1.589, Acor_av=0.829 Combined refinement in use Rint: 0.15585 There are 81 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 117 pars with 6903 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.23264 Using Levenberg-Marquardt: 0.00010 New wR= 0.05955 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15572 with corrections 0.04734 Rint for all data: 0.15585 with corrections 0.04755 0 observations identified as outliers and rejected Cycle 2 wR= 0.05955 Using Levenberg-Marquardt: 0.00001 New wR= 0.05385 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15572 with corrections 0.04223 Rint for all data: 0.15585 with corrections 0.04245 0 observations identified as outliers and rejected Cycle 3 wR= 0.05385 Using Levenberg-Marquardt: 0.00000 New wR= 0.05285 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15572 with corrections 0.04134 Rint for all data: 0.15585 with corrections 0.04156 0 observations identified as outliers and rejected Cycle 4 wR= 0.05285 Using Levenberg-Marquardt: 0.00000 New wR= 0.05234 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15572 with corrections 0.04087 Rint for all data: 0.15585 with corrections 0.04109 0 observations identified as outliers and rejected Cycle 5 wR= 0.05234 Using Levenberg-Marquardt: 0.00000 New wR= 0.05202 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.15572 with corrections 0.04056 Rint for all data: 0.15585 with corrections 0.04078 0 observations identified as outliers and rejected Final wR= 0.05202 Final frame scales: Min= 0.7488 Max= 1.3330 Final absorption correction factors: Amin= 0.4960 Amax= 1.3676 PROFFIT INFO: Inet (after scale3 abspack): min=825.0099 max=5224748.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=118.4746 max=56398.7617 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2744 reflections read from tmp file 495 reflections are rejected (494 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 5 2 1 1 6 1 9 2 81 Initial Chi^2= 0.35537 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.90540 Current error model SIG(F2)^2 = 143.15*I_RAW + 0.00*I_BACK+(0.01551*)^2 Cycle 2, Chi^2= 1.00309 Current error model SIG(F2)^2 = 104.56*I_RAW + 0.00*I_BACK+(0.01905*)^2 Cycle 3, Chi^2= 1.00017 Current error model SIG(F2)^2 = 108.35*I_RAW + 0.00*I_BACK+(0.01836*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 108.03*I_RAW + 0.00*I_BACK+(0.01843*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 108.07*I_RAW + 0.00*I_BACK+(0.01842*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 108.07*I_RAW + 0.00*I_BACK+(0.01842*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5224749- 1159252 274 1842911.07 49.88 100.00 1152314- 637481 274 845971.08 41.44 100.00 637239- 267435 274 421726.10 39.69 100.00 266913- 162784 274 202280.60 34.40 100.00 162651- 130628 274 146435.62 27.50 100.00 130520- 91565 274 106361.44 21.18 100.00 91481- 71232 274 81742.44 18.04 100.00 71214- 5111 274 41122.55 12.73 100.00 5107- 2881 274 3769.61 4.88 98.91 2878- 825 278 2241.86 3.98 82.01 ------------------------------------------------------------------------------------ 5224749- 825 2744 368920.94 25.34 98.07 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 274 765338.86 40.72 100.00 1.39- 1.12 274 678625.18 32.02 99.64 1.12- 0.96 274 424159.76 29.62 99.27 0.96- 0.88 274 359709.49 26.14 98.54 0.88- 0.81 274 446784.69 29.68 99.64 0.81- 0.73 274 233273.50 20.30 98.91 0.73- 0.71 274 174398.38 18.43 93.07 0.71- 0.65 274 309498.72 24.49 98.54 0.65- 0.62 274 152330.63 15.92 94.89 0.62- 0.58 278 148310.77 16.22 98.20 ------------------------------------------------------------------------------------ 4.82- 0.58 2744 368920.94 25.34 98.07 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 274 765338.86 40.72 100.00 4.82- 1.12 548 721982.02 36.37 99.82 4.82- 0.96 822 622707.93 34.12 99.64 4.82- 0.88 1096 556958.32 32.12 99.36 4.82- 0.81 1370 534923.59 31.64 99.42 4.82- 0.73 1644 484648.58 29.75 99.33 4.82- 0.71 1918 440327.12 28.13 98.44 4.82- 0.65 2192 423973.57 27.67 98.45 4.82- 0.62 2466 393791.02 26.37 98.05 4.82- 0.58 2744 368920.94 25.34 98.07 ------------------------------------------------------------------------------------ 4.82- 0.58 2744 368920.94 25.34 98.07 Scale applied to data: s=0.191397 (maximum obs:5224748.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.041; Rsigma 0.025: data 2744 -> merged 110 With outlier rejection... Rint 0.039; Rsigma 0.025: data 2732 -> merged 110 Rejected total: 12, method kkm 10, method Blessing 2 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585913, 4.831566 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 16.10 100.00 161 1.61 - 1.21 10 10 24.90 100.00 249 1.17 - 1.01 10 10 32.30 100.00 323 0.99 - 0.89 10 10 31.90 100.00 319 0.88 - 0.81 10 10 30.60 100.00 306 0.81 - 0.74 10 10 26.30 100.00 263 0.73 - 0.71 10 10 29.20 100.00 292 0.70 - 0.66 10 10 24.60 100.00 246 0.66 - 0.64 10 10 22.50 100.00 225 0.63 - 0.60 10 10 21.70 100.00 217 --------------------------------------------------------------- 5.92 - 0.60 100 100 26.01 100.00 2601 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:18:17 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918951 5.915618 5.915333 60.0462 90.0920 60.0327 2540 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1272 1359 1247 1282 1939 1697 1687 2540 N (int>3sigma) = 0 1009 1359 984 1025 1676 1391 1365 2061 Mean intensity = 0.0 33.4 16.1 33.7 35.7 27.5 38.2 37.4 37.2 Mean int/sigma = 0.0 22.7 19.9 22.4 22.9 21.6 24.2 23.6 23.6 Lattice type: P chosen Volume: 146.51 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Unitcell: 5.915 5.915 5.916 119.95 90.05 119.94 Niggli form: a.a = 34.984 b.b = 34.991 c.c = 34.995 b.c = -17.472 a.c = -0.033 a.b = -17.463 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.273 [ 2386] Vol = 586.1 Cell: 8.361 8.375 8.369 89.99 89.99 90.04 Volume: 586.05 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.268 [ 2109] Vol = 439.5 Cell: 5.915 5.915 14.498 89.97 90.07 119.94 Volume: 439.54 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.258 [ 673] Vol = 439.5 Trigonal Cell: 5.915 5.915 14.498 89.97 90.07 119.94 Volume: 439.54 Matrix: 0.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 -1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.071 TETRAGONAL I-lattice R(int) = 0.247 [ 2143] Vol = 293.0 Cell: 5.920 5.920 8.361 89.97 90.02 90.04 Volume: 293.03 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.056 TETRAGONAL I-lattice R(int) = 0.247 [ 2143] Vol = 293.0 Cell: 5.920 5.920 8.361 89.97 90.02 90.04 Volume: 293.03 Matrix: 1.0000 -1.0000 0.0000 0.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.025 ORTHORHOMBIC I-lattice R(int) = 0.248 [ 2089] Vol = 293.0 Cell: 5.920 8.361 5.920 89.97 89.96 89.98 Volume: 293.03 Matrix:-1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.019 MONOCLINIC I-lattice R(int) = 0.243 [ 1764] Vol = 293.0 Cell: 8.361 5.920 5.920 90.04 90.03 89.98 Volume: 293.03 Matrix:-1.0000 0.0000 -1.0000 -1.0000 1.0000 0.0000 0.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [39] err= 0.044 MONOCLINIC I-lattice R(int) = 0.241 [ 1766] Vol = 293.0 Cell: 5.916 5.915 8.375 89.97 90.02 89.95 Volume: 293.03 Matrix: 0.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 -1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.046 MONOCLINIC C-lattice R(int) = 0.229 [ 1792] Vol = 293.0 Cell: 8.361 8.375 5.915 89.97 134.97 90.04 Volume: 293.03 Matrix:-1.0000 0.0000 -1.0000 1.0000 0.0000 -1.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.210 [ 1205] Vol = 146.5 Cell: 5.915 5.915 5.916 119.95 90.05 119.94 Volume: 146.51 Matrix: 1.0000 -1.0000 1.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1359 0 1687 1697 2540 N (int>3sigma) = 0 0 0 0 1359 0 1382 1391 2061 Mean intensity = 0.0 0.0 0.0 0.0 16.1 0.0 36.8 38.2 37.2 Mean int/sigma = 0.0 0.0 0.0 0.0 19.9 0.0 23.6 24.2 23.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.173 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 25 25 186 601 N I>3s 20 20 65 601 0.4 0.4 0.4 17.6 5.7 5.7 3.2 24.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.273 2219 Fd-3m 1 1 227 C N N N N 37 2284 0.274 2257 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361382 8.374819 8.369208 89.9942 89.9911 90.0350 ZERR 1.00 0.000292 0.001681 0.003649 0.0017 0.0122 0.0013 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4329932- 544954 605 602 27 22.3 1266999.16 44.65 0.036 0.045 534840- 126420 816 814 27 30.1 224520.05 33.16 0.045 0.060 111378- 37198 679 679 27 25.1 82043.67 18.05 0.057 0.073 10722- 1863 644 637 29 22.0 3617.34 4.79 0.149 0.191 ------------------------------------------------------------------------------------------- 4329932- 1863 2744 2732 110 24.8 367315.05 25.32 0.039 0.049 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 684 676 27 25.0 655716.16 36.01 0.037 0.047 0.021 1.01-0.78 845 844 28 30.1 344627.21 24.57 0.029 0.036 0.025 0.76-0.65 730 728 28 26.0 257095.96 21.34 0.048 0.057 0.030 0.65-0.59 485 484 27 17.9 169854.07 17.71 0.066 0.073 0.038 ------------------------------------------------------------------------------------------------------ inf-0.59 2744 2732 110 24.8 367315.05 25.32 0.039 0.049 0.025 inf-0.60 2611 2599 99 26.3 380044.31 25.84 0.039 0.048 0.025 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 676 27 27 100.0 25.0 655716.16 204.93 0.037 0.006 1.01-0.78 844 28 28 100.0 30.1 344627.21 144.10 0.029 0.005 0.76-0.65 728 28 28 100.0 26.0 257095.96 115.89 0.048 0.007 0.65-0.59 484 27 27 100.0 17.9 169854.07 87.74 0.066 0.012 -------------------------------------------------------------------------------------------- inf-0.59 2732 110 110 100.0 24.8 367315.05 141.65 0.039 0.007 inf-0.60 2599 99 99 100.0 26.3 380044.31 145.36 0.039 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:24:42 2018) ID: 2932; threads 39; handles 878; mem 519568.00 (1237700.00)kB; time: 1w 5d 0h 30m 13s MEMORY INFO: Memory PF:0.0, Ph:229.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.4,peak PF: 697.1, WS: 298.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:229.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.2,peak PF: 697.1, WS: 300.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:24:42 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000012 0.000014 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) 5.91502 ( 0.00077 ) 5.91640 ( 0.00076 ) 5.92265 ( 0.00063 ) 60.05206 ( 0.01230 ) 89.98756 ( 0.00954 ) 60.01743 ( 0.01352 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:24:42 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000012 0.000013 0.000013 ) -0.068858 -0.065594 -0.010716 ( 0.000012 0.000014 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021544 -0.014366 0.007208 ( 0.000003 0.000002 0.000002 ) -0.014366 0.028731 -0.014369 ( 0.000002 0.000004 0.000002 ) 0.007208 -0.014369 0.021565 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(8) 5.9164(8) 5.9227(6) 60.052(12) 89.988(9) 60.017(14) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.973 ( 0.161) | 1.251 ( 0.602) | 1.661 ( 2.344) | 1.33- 1.09 | 44 | 1.060 ( 0.121) | 1.083 ( 0.154) | 1.091 ( 0.488) | 1.09- 0.96 | 44 | 1.056 ( 0.111) | 1.071 ( 0.138) | 1.092 ( 0.416) | 0.94- 0.84 | 44 | 1.083 ( 0.108) | 1.073 ( 0.135) | 1.145 ( 0.399) | 0.84- 0.81 | 44 | 1.105 ( 0.099) | 1.023 ( 0.124) | 1.367 ( 0.511) | 0.81- 0.73 | 44 | 1.095 ( 0.086) | 0.996 ( 0.125) | 1.322 ( 0.491) | 0.73- 0.69 | 44 | 1.089 ( 0.080) | 0.930 ( 0.110) | 1.402 ( 0.496) | 0.69- 0.66 | 44 | 1.080 ( 0.074) | 0.883 ( 0.089) | 1.388 ( 0.489) | 0.66- 0.63 | 44 | 1.059 ( 0.070) | 0.859 ( 0.064) | 1.418 ( 0.589) | 0.63- 0.59 | 45 | 1.018 ( 0.090) | 0.818 ( 0.077) | 1.291 ( 0.549) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 441 | 1.062 ( 0.110) | 0.998 ( 0.252) | 1.318 ( 0.893) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.070035 0.030486 0.088658 ( 0.000027 0.000026 0.000015 ) -0.068374 -0.065763 -0.010700 ( 0.000027 0.000027 0.000015 ) 0.109065 -0.152749 0.115659 ( 0.000027 0.000027 0.000015 ) M - matrix: 0.021475 -0.014298 0.007137 ( 0.000008 0.000006 0.000005 ) -0.014298 0.028586 -0.014260 ( 0.000006 0.000009 0.000005 ) 0.007137 -0.014260 0.021352 ( 0.000005 0.000005 0.000004 ) unit cell: 5.9266(15) 5.9308(15) 5.9444(11) 60.01(2) 90.017(18) 60.02(3) V = 147.80(5) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 UB - matrix: -0.070138 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9215(14) 5.9313(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070138 0.030665 0.088728 ( 0.000024 0.000024 0.000014 ) -0.068207 -0.065969 -0.010733 ( 0.000025 0.000025 0.000014 ) 0.109141 -0.153002 0.116013 ( 0.000024 0.000023 0.000014 ) M - matrix: 0.021483 -0.014350 0.007171 ( 0.000007 0.000005 0.000004 ) -0.014350 0.028702 -0.014321 ( 0.000005 0.000008 0.000004 ) 0.007171 -0.014321 0.021447 ( 0.000004 0.000004 0.000004 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 5.9297(14) 5.9215(14) 5.9313(10) 60.04(2) 90.041(16) 59.98(2) V = 147.25(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 448 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.980 ( 0.168) | 1.292 ( 0.707) | 1.567 ( 2.300) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.170 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.142) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.029 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.993 ( 0.128) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.383 ( 0.483) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 44 | 1.006 ( 0.077) | 0.807 ( 0.033) | 1.274 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 440 | 1.063 ( 0.108) | 1.004 ( 0.281) | 1.323 ( 0.875) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 484 peaks identified as outliers and rejected 474 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 474 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 474 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.032 ( 0.144) | 1.122 ( 0.424) | 1.109 ( 0.575) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.275 ( 0.643) | 1.092 ( 0.634) | 1.12- 0.98 | 47 | 1.019 ( 0.102) | 1.057 ( 0.160) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.029 ( 0.093) | 1.035 ( 0.135) | 1.097 ( 0.433) | 0.89- 0.82 | 47 | 1.036 ( 0.085) | 1.007 ( 0.124) | 1.151 ( 0.478) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.196 ( 0.514) | 0.75- 0.71 | 47 | 1.027 ( 0.045) | 0.938 ( 0.113) | 1.296 ( 0.513) | 0.71- 0.67 | 47 | 1.001 ( 0.040) | 0.889 ( 0.071) | 1.260 ( 0.499) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.301 ( 0.513) | 0.63- 0.59 | 51 | 0.945 ( 0.054) | 0.815 ( 0.041) | 1.344 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 474 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.182 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088653 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010206 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116127 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.014 ( 0.108) | 1.028 ( 0.130) | 0.949 ( 0.328) | 0.97- 0.89 | 47 | 1.028 ( 0.089) | 1.029 ( 0.137) | 1.105 ( 0.406) | 0.88- 0.82 | 47 | 1.047 ( 0.079) | 1.022 ( 0.118) | 1.207 ( 0.509) | 0.82- 0.75 | 47 | 1.037 ( 0.080) | 0.987 ( 0.126) | 1.069 ( 0.407) | 0.75- 0.71 | 47 | 1.022 ( 0.044) | 0.934 ( 0.110) | 1.339 ( 0.543) | 0.71- 0.67 | 47 | 0.997 ( 0.043) | 0.885 ( 0.072) | 1.211 ( 0.465) | 0.67- 0.63 | 47 | 0.974 ( 0.047) | 0.841 ( 0.041) | 1.288 ( 0.498) | 0.63- 0.59 | 49 | 0.949 ( 0.045) | 0.812 ( 0.041) | 1.347 ( 0.519) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 472 | 1.014 ( 0.090) | 0.993 ( 0.294) | 1.173 ( 0.533) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb PROFFITPEAK info: 816 peaks in the peak location table UB fit with 377 obs out of 399 (total:399,skipped:0) (94.49%) UB - matrix: -0.069456 0.031075 0.089070 ( 0.000049 0.000085 0.000093 ) -0.069022 -0.065413 -0.010153 ( 0.000033 0.000057 0.000063 ) 0.108897 -0.152935 0.116106 ( 0.000059 0.000103 0.000112 ) M - matrix: 0.021447 -0.014298 0.007158 ( 0.000015 0.000016 0.000017 ) -0.014298 0.028634 -0.014325 ( 0.000016 0.000033 0.000023 ) 0.007158 -0.014325 0.021517 ( 0.000017 0.000023 0.000031 ) unit cell: 5.930(3) 5.925(3) 5.921(4) 60.02(7) 90.02(5) 60.03(6) V = 147.17(15) UB fit with 377 obs out of 399 (total:399,skipped:0) (94.49%) UB - matrix: -0.069456 0.031075 0.089070 ( 0.000049 0.000085 0.000093 ) -0.069022 -0.065413 -0.010153 ( 0.000033 0.000057 0.000063 ) 0.108897 -0.152935 0.116106 ( 0.000059 0.000103 0.000112 ) M - matrix: 0.021447 -0.014298 0.007158 ( 0.000015 0.000016 0.000017 ) -0.014298 0.028634 -0.014325 ( 0.000016 0.000033 0.000023 ) 0.007158 -0.014325 0.021517 ( 0.000017 0.000023 0.000031 ) unit cell: 5.930(3) 5.925(3) 5.921(4) 60.02(7) 90.02(5) 60.03(6) V = 147.17(15) OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 UB - matrix: -0.069568 0.031287 0.088956 ( 0.000051 0.000089 0.000096 ) -0.068811 -0.065484 -0.010024 ( 0.000034 0.000060 0.000065 ) 0.108961 -0.152834 0.116174 ( 0.000060 0.000104 0.000113 ) M - matrix: 0.021447 -0.014324 0.007160 ( 0.000016 0.000017 0.000017 ) -0.014324 0.028625 -0.014316 ( 0.000017 0.000033 0.000023 ) 0.007160 -0.014316 0.021510 ( 0.000017 0.000023 0.000031 ) UB fit with 380 obs out of 399 (total:399,skipped:0) (95.24%) unit cell: 5.936(4) 5.930(3) 5.921(4) 60.04(7) 89.99(5) 59.94(6) V = 147.34(15) UB fit with 380 obs out of 399 (total:399,skipped:0) (95.24%) UB - matrix: -0.069568 0.031287 0.088956 ( 0.000051 0.000089 0.000096 ) -0.068811 -0.065484 -0.010024 ( 0.000034 0.000060 0.000065 ) 0.108961 -0.152834 0.116174 ( 0.000060 0.000104 0.000113 ) M - matrix: 0.021447 -0.014324 0.007160 ( 0.000016 0.000017 0.000017 ) -0.014324 0.028625 -0.014316 ( 0.000017 0.000033 0.000023 ) 0.007160 -0.014316 0.021510 ( 0.000017 0.000023 0.000031 ) unit cell: 5.936(4) 5.930(3) 5.921(4) 60.04(7) 89.99(5) 59.94(6) V = 147.34(15) OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 OTKP changes: 74 1 1 1 UB - matrix: -0.069570 0.031296 0.088947 ( 0.000051 0.000089 0.000096 ) -0.068797 -0.065489 -0.010015 ( 0.000034 0.000060 0.000065 ) 0.108964 -0.152830 0.116169 ( 0.000060 0.000104 0.000113 ) M - matrix: 0.021446 -0.014325 0.007159 ( 0.000016 0.000017 0.000017 ) -0.014325 0.028625 -0.014314 ( 0.000017 0.000033 0.000023 ) 0.007159 -0.014314 0.021507 ( 0.000017 0.000023 0.000031 ) UB fit with 380 obs out of 399 (total:399,skipped:0) (95.24%) unit cell: 5.936(4) 5.931(3) 5.921(4) 60.04(7) 89.98(5) 59.93(6) V = 147.36(15) 399 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Run 5 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 585 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069570 0.031296 0.088947 ( 0.000051 0.000089 0.000096 ) -0.068797 -0.065489 -0.010015 ( 0.000034 0.000060 0.000065 ) 0.108964 -0.152830 0.116169 ( 0.000060 0.000104 0.000113 ) M - matrix: 0.021446 -0.014325 0.007159 ( 0.000016 0.000017 0.000017 ) -0.014325 0.028625 -0.014314 ( 0.000017 0.000033 0.000023 ) 0.007159 -0.014314 0.021507 ( 0.000017 0.000023 0.000031 ) UB fit with 380 obs out of 399 (total:399,skipped:0) (95.24%) unit cell: 5.936(4) 5.931(3) 5.921(4) 60.04(7) 89.98(5) 59.93(6) V = 147.36(15) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 379 obs out of 399 (total:399,skipped:0) (94.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb 3 of 335 peaks identified as outliers and rejected 332 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 332 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 332 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.48 | 33 | 1.017 ( 0.207) | 1.313 ( 0.733) | 1.133 ( 0.699) | 1.47- 1.17 | 33 | 1.026 ( 0.086) | 1.046 ( 0.115) | 0.969 ( 0.383) | 1.17- 0.99 | 33 | 0.999 ( 0.091) | 1.004 ( 0.123) | 0.961 ( 0.399) | 0.98- 0.92 | 33 | 1.004 ( 0.076) | 1.007 ( 0.115) | 1.091 ( 0.451) | 0.92- 0.82 | 33 | 1.009 ( 0.065) | 0.962 ( 0.094) | 1.286 ( 0.504) | 0.82- 0.76 | 33 | 1.012 ( 0.082) | 0.962 ( 0.110) | 1.241 ( 0.467) | 0.76- 0.71 | 33 | 0.979 ( 0.048) | 0.928 ( 0.070) | 1.265 ( 0.442) | 0.71- 0.67 | 33 | 0.954 ( 0.043) | 0.878 ( 0.063) | 1.299 ( 0.524) | 0.67- 0.63 | 33 | 0.929 ( 0.037) | 0.839 ( 0.029) | 1.428 ( 0.474) | 0.62- 0.59 | 35 | 0.894 ( 0.034) | 0.808 ( 0.032) | 1.431 ( 0.605) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 332 | 0.982 ( 0.100) | 0.974 ( 0.281) | 1.212 ( 0.528) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 332 obs out of 332 (total:332,skipped:0) (100.00%) UB - matrix: -0.069834 0.031361 0.088962 ( 0.000021 0.000037 0.000038 ) -0.068916 -0.065450 -0.010129 ( 0.000019 0.000033 0.000034 ) 0.109182 -0.152927 0.116334 ( 0.000021 0.000037 0.000038 ) M - matrix: 0.021547 -0.014376 0.007187 ( 0.000006 0.000006 0.000006 ) -0.014376 0.028654 -0.014338 ( 0.000006 0.000012 0.000008 ) 0.007187 -0.014338 0.021551 ( 0.000006 0.000008 0.000011 ) unit cell: 5.9244(17) 5.9299(17) 5.9157(17) 60.04(3) 89.97(2) 59.90(3) V = 146.86(7) OTKP changes: 332 1 1 1 OTKP changes: 332 1 1 1 OTKP changes: 332 1 1 1 UB - matrix: -0.069571 0.031207 0.088971 ( 0.000020 0.000035 0.000036 ) -0.068947 -0.065427 -0.010100 ( 0.000018 0.000033 0.000033 ) 0.109029 -0.152993 0.116173 ( 0.000017 0.000031 0.000032 ) M - matrix: 0.021481 -0.014341 0.007173 ( 0.000005 0.000006 0.000006 ) -0.014341 0.028661 -0.014336 ( 0.000006 0.000011 0.000007 ) 0.007173 -0.014336 0.021514 ( 0.000006 0.000007 0.000010 ) UB fit with 332 obs out of 332 (total:332,skipped:0) (100.00%) unit cell: 5.9303(17) 5.9275(16) 5.9226(16) 60.01(3) 90.00(2) 59.96(3) V = 147.15(6) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 584 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069571 0.031207 0.088971 ( 0.000020 0.000035 0.000036 ) -0.068947 -0.065427 -0.010100 ( 0.000018 0.000033 0.000033 ) 0.109029 -0.152993 0.116173 ( 0.000017 0.000031 0.000032 ) M - matrix: 0.021481 -0.014341 0.007173 ( 0.000005 0.000006 0.000006 ) -0.014341 0.028661 -0.014336 ( 0.000006 0.000011 0.000007 ) 0.007173 -0.014336 0.021514 ( 0.000006 0.000007 0.000010 ) UB fit with 332 obs out of 332 (total:332,skipped:0) (100.00%) unit cell: 5.9303(17) 5.9275(16) 5.9226(16) 60.01(3) 90.00(2) 59.96(3) V = 147.15(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 332 obs out of 332 (total:332,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb 3 of 338 peaks identified as outliers and rejected 335 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 335 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 335 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.48 | 34 | 1.019 ( 0.211) | 1.215 ( 0.661) | 1.209 ( 0.825) | 1.42- 1.17 | 34 | 1.023 ( 0.087) | 1.041 ( 0.115) | 0.972 ( 0.382) | 1.16- 0.99 | 34 | 0.997 ( 0.095) | 1.019 ( 0.127) | 0.984 ( 0.423) | 0.99- 0.92 | 34 | 1.008 ( 0.070) | 1.004 ( 0.106) | 1.082 ( 0.447) | 0.92- 0.82 | 34 | 1.004 ( 0.072) | 0.957 ( 0.107) | 1.298 ( 0.485) | 0.82- 0.76 | 34 | 1.010 ( 0.081) | 0.961 ( 0.107) | 1.236 ( 0.464) | 0.75- 0.71 | 34 | 0.980 ( 0.048) | 0.927 ( 0.066) | 1.303 ( 0.474) | 0.71- 0.67 | 34 | 0.956 ( 0.044) | 0.872 ( 0.063) | 1.269 ( 0.552) | 0.67- 0.63 | 34 | 0.917 ( 0.031) | 0.836 ( 0.028) | 1.496 ( 0.455) | 0.63- 0.59 | 29 | 0.892 ( 0.035) | 0.803 ( 0.031) | 1.399 ( 0.646) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 335 | 0.982 ( 0.101) | 0.966 ( 0.253) | 1.222 ( 0.552) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 213 | 1.119 ( 0.126) | 1.220 ( 0.427) | 1.237 ( 1.160) | 13.2-19.0 | 213 | 1.079 ( 0.054) | 1.133 ( 0.283) | 1.195 ( 0.521) | 19.0-23.1 | 214 | 1.068 ( 0.071) | 1.151 ( 0.408) | 1.199 ( 0.543) | 23.1-27.2 | 213 | 1.034 ( 0.077) | 1.066 ( 0.262) | 1.183 ( 0.565) | 27.2-30.7 | 213 | 1.011 ( 0.071) | 1.007 ( 0.241) | 1.192 ( 0.491) | 30.7-33.8 | 213 | 0.981 ( 0.081) | 0.920 ( 0.104) | 1.200 ( 0.513) | 33.8-36.9 | 214 | 0.962 ( 0.074) | 0.903 ( 0.108) | 1.186 ( 0.483) | 36.9-39.6 | 213 | 0.947 ( 0.086) | 0.869 ( 0.133) | 1.225 ( 0.555) | 39.6-42.7 | 213 | 0.923 ( 0.074) | 0.836 ( 0.078) | 1.190 ( 0.536) | 42.7-49.9 | 213 | 0.928 ( 0.085) | 0.811 ( 0.065) | 1.152 ( 0.474) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2132 | 1.005 ( 0.104) | 0.992 ( 0.282) | 1.196 ( 0.616) | Fitted profile normalization line parameters e1 dimension: a=-0.0047 b=1.16 e2 dimension: a=-0.0097 b=1.26 e3 dimension: a=0.0025 b=1.00 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706998 Maximum peak integral for reflections I/sig<= 10000 - raw: 10984832 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:25:05 2018 PROFFITMAIN - Started at Tue Mar 27 15:25:05 2018 OTKP changes: 2132 2 4 5 OTKP changes: 2132 2 4 5 UB - matrix: -0.070080 0.031143 0.088946 ( 0.000011 0.000013 0.000012 ) -0.068748 -0.065903 -0.010397 ( 0.000010 0.000012 0.000011 ) 0.109169 -0.153056 0.116351 ( 0.000009 0.000011 0.000010 ) M - matrix: 0.021555 -0.014361 0.007183 ( 0.000003 0.000002 0.000002 ) -0.014361 0.028739 -0.014353 ( 0.000002 0.000004 0.000002 ) 0.007183 -0.014353 0.021557 ( 0.000002 0.000002 0.000003 ) UB fit with 2132 obs out of 2132 (total:2132,skipped:0) (100.00%) unit cell: 5.9151(7) 5.9118(7) 5.9131(6) 60.057(11) 90.045(9) 60.028(12) V = 146.34(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) UB - matrix: -0.070057 0.030669 0.088948 ( 0.000028 0.000028 0.000016 ) -0.068240 -0.066132 -0.010522 ( 0.000025 0.000025 0.000014 ) 0.109077 -0.153060 0.115984 ( 0.000025 0.000024 0.000014 ) M - matrix: 0.021462 -0.014331 0.007138 ( 0.000007 0.000006 0.000004 ) -0.014331 0.028741 -0.014329 ( 0.000006 0.000008 0.000004 ) 0.007138 -0.014329 0.021475 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9280(14) 5.9140(14) 5.9250(11) 60.02(2) 89.972(18) 60.00(2) V = 146.95(5) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 UB - matrix: -0.070359 0.030958 0.088811 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066158 -0.010654 ( 0.000024 0.000023 0.000013 ) 0.109356 -0.153298 0.116379 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021588 -0.014417 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014417 0.028835 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014386 0.021545 ( 0.000004 0.000004 0.000004 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 5.9148(13) 5.9069(13) 5.9175(10) 60.05(2) 90.057(16) 59.99(2) V = 146.20(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.778) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070359 0.030958 0.088811 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066158 -0.010654 ( 0.000024 0.000023 0.000013 ) 0.109356 -0.153298 0.116379 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021588 -0.014417 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014417 0.028835 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014386 0.021545 ( 0.000004 0.000004 0.000004 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 5.9148(13) 5.9069(13) 5.9175(10) 60.05(2) 90.057(16) 59.99(2) V = 146.20(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070359 0.030958 0.088811 ( 0.000026 0.000026 0.000015 ) -0.068405 -0.066158 -0.010654 ( 0.000024 0.000023 0.000013 ) 0.109356 -0.153298 0.116379 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021588 -0.014417 0.007207 ( 0.000007 0.000005 0.000004 ) -0.014417 0.028835 -0.014386 ( 0.000005 0.000008 0.000004 ) 0.007207 -0.014386 0.021545 ( 0.000004 0.000004 0.000004 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 5.9148(13) 5.9069(13) 5.9175(10) 60.05(2) 90.057(16) 59.99(2) V = 146.20(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070406 0.031337 0.088630 ( 0.000025 0.000022 0.000027 ) -0.068581 -0.065990 -0.010248 ( 0.000031 0.000027 0.000033 ) 0.108994 -0.152665 0.116253 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021540 -0.014320 0.007134 ( 0.000007 0.000005 0.000005 ) -0.014320 0.028643 -0.014294 ( 0.000005 0.000006 0.000005 ) 0.007134 -0.014294 0.021475 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(16) 5.9212(16) 5.9228(13) 60.03(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070374 0.031241 0.088845 ( 0.000023 0.000020 0.000025 ) -0.068817 -0.065843 -0.010374 ( 0.000030 0.000026 0.000032 ) 0.109171 -0.153160 0.116603 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021607 -0.014388 0.007191 ( 0.000007 0.000005 0.000005 ) -0.014388 0.028769 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007191 -0.014400 0.021597 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9086(16) 5.9155(16) 5.9130(12) 59.95(2) 89.957(19) 60.01(3) V = 146.10(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.778) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070374 0.031241 0.088845 ( 0.000023 0.000020 0.000025 ) -0.068817 -0.065843 -0.010374 ( 0.000030 0.000026 0.000032 ) 0.109171 -0.153160 0.116603 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021607 -0.014388 0.007191 ( 0.000007 0.000005 0.000005 ) -0.014388 0.028769 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007191 -0.014400 0.021597 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9086(16) 5.9155(16) 5.9130(12) 59.95(2) 89.957(19) 60.01(3) V = 146.10(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070374 0.031241 0.088845 ( 0.000023 0.000020 0.000025 ) -0.068817 -0.065843 -0.010374 ( 0.000030 0.000026 0.000032 ) 0.109171 -0.153160 0.116603 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021607 -0.014388 0.007191 ( 0.000007 0.000005 0.000005 ) -0.014388 0.028769 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007191 -0.014400 0.021597 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9086(16) 5.9155(16) 5.9130(12) 59.95(2) 89.957(19) 60.01(3) V = 146.10(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) UB - matrix: -0.070142 0.031467 0.088649 ( 0.000016 0.000025 0.000021 ) -0.068849 -0.065715 -0.010176 ( 0.000020 0.000032 0.000027 ) 0.108932 -0.152889 0.116166 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021526 -0.014337 0.007137 ( 0.000005 0.000005 0.000004 ) -0.014337 0.028684 -0.014302 ( 0.000005 0.000009 0.000005 ) 0.007137 -0.014302 0.021457 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9191(15) 5.9194(15) 5.9262(11) 60.03(2) 89.952(18) 59.98(3) V = 146.91(5) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 UB - matrix: -0.070163 0.031462 0.088883 ( 0.000016 0.000025 0.000021 ) -0.068737 -0.066038 -0.009947 ( 0.000018 0.000028 0.000024 ) 0.109191 -0.153141 0.116592 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021570 -0.014390 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014390 0.028803 -0.014402 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014402 0.021593 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9147(13) 5.9126(14) 5.9125(11) 59.96(2) 89.934(17) 59.98(2) V = 146.15(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.778) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070163 0.031462 0.088883 ( 0.000016 0.000025 0.000021 ) -0.068737 -0.066038 -0.009947 ( 0.000018 0.000028 0.000024 ) 0.109191 -0.153141 0.116592 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021570 -0.014390 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014390 0.028803 -0.014402 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014402 0.021593 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9147(13) 5.9126(14) 5.9125(11) 59.96(2) 89.934(17) 59.98(2) V = 146.15(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070163 0.031462 0.088883 ( 0.000016 0.000025 0.000021 ) -0.068737 -0.066038 -0.009947 ( 0.000018 0.000028 0.000024 ) 0.109191 -0.153141 0.116592 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021570 -0.014390 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014390 0.028803 -0.014402 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014402 0.021593 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9147(13) 5.9126(14) 5.9125(11) 59.96(2) 89.934(17) 59.98(2) V = 146.15(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 335 obs out of 335 (total:335,skipped:0) (100.00%) UB - matrix: -0.069803 0.031332 0.088967 ( 0.000020 0.000036 0.000037 ) -0.068948 -0.065431 -0.010138 ( 0.000018 0.000032 0.000033 ) 0.109164 -0.152946 0.116317 ( 0.000020 0.000036 0.000037 ) M - matrix: 0.021543 -0.014372 0.007186 ( 0.000006 0.000006 0.000006 ) -0.014372 0.028656 -0.014340 ( 0.000006 0.000012 0.000008 ) 0.007186 -0.014340 0.021548 ( 0.000006 0.000008 0.000011 ) unit cell: 5.9242(17) 5.9294(17) 5.9166(17) 60.03(3) 89.98(2) 59.91(3) V = 146.87(6) OTKP changes: 335 1 1 1 OTKP changes: 335 1 1 1 OTKP changes: 335 1 1 1 UB - matrix: -0.069902 0.031362 0.089079 ( 0.000019 0.000034 0.000035 ) -0.069115 -0.065528 -0.010300 ( 0.000017 0.000031 0.000032 ) 0.109181 -0.153392 0.116519 ( 0.000018 0.000031 0.000032 ) M - matrix: 0.021584 -0.014411 0.007207 ( 0.000005 0.000006 0.000006 ) -0.014411 0.028807 -0.014404 ( 0.000006 0.000011 0.000007 ) 0.007207 -0.014404 0.021618 ( 0.000006 0.000007 0.000010 ) UB fit with 335 obs out of 335 (total:335,skipped:0) (100.00%) unit cell: 5.9161(16) 5.9118(16) 5.9077(16) 60.02(3) 90.00(2) 59.96(3) V = 146.06(6) Run 5 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.778) HKL list info: 577 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069902 0.031362 0.089079 ( 0.000019 0.000034 0.000035 ) -0.069115 -0.065528 -0.010300 ( 0.000017 0.000031 0.000032 ) 0.109181 -0.153392 0.116519 ( 0.000018 0.000031 0.000032 ) M - matrix: 0.021584 -0.014411 0.007207 ( 0.000005 0.000006 0.000006 ) -0.014411 0.028807 -0.014404 ( 0.000006 0.000011 0.000007 ) 0.007207 -0.014404 0.021618 ( 0.000006 0.000007 0.000010 ) UB fit with 335 obs out of 335 (total:335,skipped:0) (100.00%) unit cell: 5.9161(16) 5.9118(16) 5.9077(16) 60.02(3) 90.00(2) 59.96(3) V = 146.06(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 335 obs out of 335 (total:335,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.069902 0.031362 0.089079 ( 0.000019 0.000034 0.000035 ) -0.069115 -0.065528 -0.010300 ( 0.000017 0.000031 0.000032 ) 0.109181 -0.153392 0.116519 ( 0.000018 0.000031 0.000032 ) M - matrix: 0.021584 -0.014411 0.007207 ( 0.000005 0.000006 0.000006 ) -0.014411 0.028807 -0.014404 ( 0.000006 0.000011 0.000007 ) 0.007207 -0.014404 0.021618 ( 0.000006 0.000007 0.000010 ) UB fit with 335 obs out of 335 (total:335,skipped:0) (100.00%) unit cell: 5.9161(16) 5.9118(16) 5.9077(16) 60.02(3) 90.00(2) 59.96(3) V = 146.06(6) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.069980 0.031122 0.088909 ( 0.000011 0.000013 0.000012 ) -0.068791 -0.065790 -0.010445 ( 0.000012 0.000014 0.000013 ) 0.109161 -0.153094 0.116429 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021545 -0.014364 0.007206 ( 0.000003 0.000002 0.000002 ) -0.014364 0.028735 -0.014370 ( 0.000002 0.000004 0.000002 ) 0.007206 -0.014370 0.021570 ( 0.000002 0.000002 0.000003 ) UB fit with 2132 obs out of 2132 (total:2132,skipped:0) (100.00%) unit cell: 5.9180(7) 5.9145(7) 5.9143(6) 60.046(12) 90.090(9) 60.040(13) V = 146.46(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 62 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof 2892 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:25:10 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.778) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.778) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.778) Run 5 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.778) PROFFIT INFO: signal sum: min=235.0000 max=20919086.0000 PROFFIT INFO: signal sum lp corr: min=473.0593 max=2975269.4472 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=756.8949 max=4760431.5000 PROFFIT INFO: sig(Inet): min=121.7004 max=47816.8594 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 30 139 304 592 666 1177 1931 2651 2892 Percent 0.0 0.0 1.0 4.8 10.5 20.5 23.0 40.7 66.8 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2892 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2892 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4760432- 1137875 289 1878248.64 121.87 100.00 1137848- 636838 289 865395.21 103.65 100.00 635920- 269029 289 421491.59 95.68 100.00 268714- 172101 289 205000.67 70.28 100.00 172040- 121576 289 146923.42 51.14 100.00 121562- 94982 289 107414.55 36.40 100.00 94870- 67683 289 82425.88 29.79 100.00 67570- 5611 289 37511.33 19.03 100.00 5597- 2977 289 3964.19 5.37 96.89 2972- 757 291 2139.86 3.72 55.33 ------------------------------------------------------------------------------------ 4760432- 757 2892 374793.64 53.66 95.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 289 655004.11 86.74 99.31 1.32- 1.05 289 577090.00 67.77 97.58 1.05- 0.92 289 459113.06 61.49 98.27 0.92- 0.81 289 336230.82 52.21 94.46 0.81- 0.73 289 434024.46 58.75 96.19 0.73- 0.67 289 361213.75 56.03 96.54 0.67- 0.61 289 204018.55 37.56 93.43 0.61- 0.56 289 303262.00 45.78 92.39 0.56- 0.51 289 227296.69 37.82 90.31 0.51- 0.40 291 191948.33 32.60 93.47 ------------------------------------------------------------------------------------ 5.26- 0.40 2892 374793.64 53.66 95.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:25:11 2018 Sorting 2892 observations 295 unique observations with > 7.00 F2/sig(F2) 2892 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 73 494 Total number of frames 494 Maximum number of 295 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 2892 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 36 250 Total number of frames 250 2323 observations > 7.00 F2/sig(F2) 2323 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 36 250 Total number of frames 250 Removing 'redundancy=1' reflections Average redundancy: 8.1 (Out of 2323 removed 25 = 2298, unique = 282) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2298 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 36 250 Total number of frames 250 282 unique data precomputed (should be 282) 282 unique data with 2298 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.1 (Out of 2298 removed 0 = 2298, unique = 282) 282 unique data precomputed (should be 282) 282 unique data with 2298 observations RMS deviation of equivalent data = 0.73114 Rint = 0.69645 12 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.67952, wR= 3.79231 Trying model 1 (ne=2, no=0)... Results: Rint= 0.69243, wR= 2.99755, Acormin=0.113, Acormax=1.923, Acor_av=0.824 F test: Probability=0.000, F= 0.961 Trying model 2 (ne=2, no=1)... Results: Rint= 0.76369, wR= 2.92231, Acormin=-0.385, Acormax=1.901, Acor_av=0.664 F test: Probability=0.000, F= 0.789 Trying model 3 (ne=4, no=0)... Results: Rint= 0.73594, wR= 2.67461, Acormin=-0.147, Acormax=2.190, Acor_av=0.698 F test: Probability=0.000, F= 0.847 Trying model 4 (ne=4, no=1)... Results: Rint= 0.80765, wR= 2.60782, Acormin=-0.492, Acormax=1.890, Acor_av=0.559 F test: Probability=0.000, F= 0.702 Trying model 5 (ne=4, no=3)... Results: Rint= 0.82771, wR= 2.64097, Acormin=-0.919, Acormax=2.042, Acor_av=0.447 F test: Probability=0.000, F= 0.666 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75901, wR= 2.62529, Acormin=-0.412, Acormax=2.618, Acor_av=0.628 F test: Probability=0.000, F= 0.791 Trying model 7 (ne=6, no=1)... Results: Rint= 0.82119, wR= 2.64210, Acormin=-0.738, Acormax=2.146, Acor_av=0.479 F test: Probability=0.000, F= 0.674 Trying model 8 (ne=6, no=3)... Results: Rint= 0.84854, wR= 2.62476, Acormin=-1.290, Acormax=1.911, Acor_av=0.376 F test: Probability=0.000, F= 0.629 Trying model 9 (ne=6, no=5)... Results: Rint= 0.86602, wR= 2.62598, Acormin=-1.105, Acormax=2.216, Acor_av=0.319 F test: Probability=0.000, F= 0.601 Trying model 10 (ne=8, no=0)... Results: Rint= 0.83418, wR= 2.31150, Acormin=-0.697, Acormax=2.199, Acor_av=0.440 F test: Probability=0.000, F= 0.649 Trying model 11 (ne=8, no=1)... Results: Rint= 0.89818, wR= 2.00829, Acormin=-1.030, Acormax=1.562, Acor_av=0.224 F test: Probability=0.000, F= 0.559 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98809, wR= 1.67771, Acormin=-0.047, Acormax=0.067, Acor_av=0.002 F test: Probability=0.000, F= 0.460 Trying model 13 (ne=8, no=5)... Results: Rint= 0.99032, wR= 1.67052, Acormin=-0.045, Acormax=0.069, Acor_av=0.002 F test: Probability=0.000, F= 0.456 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00557, wR= 1.77150, Acormin=-0.041, Acormax=0.070, Acor_av=0.002 F test: Probability=0.000, F= 0.438 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86524 There are 250 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 254 pars with 32385 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.73114 Using Levenberg-Marquardt: 0.00010 New wR= 0.70967 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.69645 with corrections 0.67394 Rint for all data: 0.86524 with corrections 0.84798 15 observations identified as outliers and rejected Cycle 2 wR= 0.68476 Using Levenberg-Marquardt: 0.00001 New wR= 0.68222 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67484 with corrections 0.65349 Rint for all data: 0.86524 with corrections 0.85143 11 observations identified as outliers and rejected Cycle 3 wR= 0.65938 Using Levenberg-Marquardt: 0.00000 New wR= 0.65843 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66477 with corrections 0.66110 Rint for all data: 0.86524 with corrections 0.86240 8 observations identified as outliers and rejected Cycle 4 wR= 0.64545 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.63748 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66037 with corrections 0.66038 Rint for all data: 0.86524 with corrections 0.86463 3 observations identified as outliers and rejected Cycle 5 wR= 0.63126 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64327 Using Levenberg-Marquardt: 0.10000 New wR= 0.63047 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65833 with corrections 0.66002 Rint for all data: 0.86524 with corrections 0.86503 6 observations identified as outliers and rejected Final wR= 0.63047 Final frame scales: Min= 1.0000 Max= 7.9807 Final absorption correction factors: Amin= 0.1991 Amax= 1.7546 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 250 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 254 pars with 32385 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.85348 Using Levenberg-Marquardt: 0.00010 New wR= 0.85863 Using Levenberg-Marquardt: 0.00100 New wR= 0.82094 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65494 with corrections 1.45506 Rint for all data: 0.86524 with corrections 1.52853 2 observations identified as outliers and rejected Cycle 2 wR= 0.81248 Using Levenberg-Marquardt: 0.00010 New wR= 0.69235 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65428 with corrections 1.75734 Rint for all data: 0.86524 with corrections 1.76887 4 observations identified as outliers and rejected Cycle 3 wR= 0.68549 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.62738 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65363 with corrections 0.95460 Rint for all data: 0.86524 with corrections 1.08945 0 observations identified as outliers and rejected Cycle 4 wR= 0.62738 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.61984 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65363 with corrections 0.73325 Rint for all data: 0.86524 with corrections 0.91430 0 observations identified as outliers and rejected Cycle 5 wR= 0.61984 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.61079 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65363 with corrections 0.68336 Rint for all data: 0.86524 with corrections 0.88063 0 observations identified as outliers and rejected Final wR= 0.61079 Final frame scales: Min= 1.0000 Max= 19.1693 Final absorption correction factors: Amin= 0.1673 Amax= 1.6779 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 28 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 32 pars with 528 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.91880 Using Levenberg-Marquardt: 0.00010 New wR= 0.85893 There are 6 clusters with unrefined scales (size 2-54) Rint for refined data: 0.65363 with corrections 1.34760 Rint for all data: 0.86524 with corrections 1.42186 7 observations identified as outliers and rejected Cycle 2 wR= 0.88476 Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.88316 There are 6 clusters with unrefined scales (size 2-54) Rint for refined data: 0.65184 with corrections 1.30598 Rint for all data: 0.86524 with corrections 1.38979 3 observations identified as outliers and rejected Cycle 3 wR= 0.88329 Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.88158 There are 6 clusters with unrefined scales (size 2-54) Rint for refined data: 0.65047 with corrections 1.43814 Rint for all data: 0.86524 with corrections 1.51725 2 observations identified as outliers and rejected Cycle 4 wR= 0.88114 Using Levenberg-Marquardt: 1.00000 New wR= 0.87887 There are 6 clusters with unrefined scales (size 2-54) Rint for refined data: 0.64844 with corrections 1.21386 Rint for all data: 0.86524 with corrections 1.28243 2 observations identified as outliers and rejected Cycle 5 wR= 0.87787 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 10.00000 New wR= 0.87645 There are 6 clusters with unrefined scales (size 2-54) Rint for refined data: 0.64833 with corrections 1.31570 Rint for all data: 0.86524 with corrections 1.37543 1 observations identified as outliers and rejected Final wR= 0.87645 Frame scales out of range! Absorption correction factors out of range! Negative absorption correction factors! Trying with lower orders of spherical harmonics Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 11 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Refinement control: 10 pars with 55 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.97981 Using Levenberg-Marquardt: 0.00010 New wR= 0.71541 There are 5 clusters with unrefined scales (size 34-55) Rint for refined data: 0.64819 with corrections 0.74121 Rint for all data: 0.86524 with corrections 0.95257 7 observations identified as outliers and rejected Cycle 2 wR= 0.86220 Using Levenberg-Marquardt: 0.00001 New wR= 0.85997 There are 5 clusters with unrefined scales (size 34-55) Rint for refined data: 0.64526 with corrections 0.72443 Rint for all data: 0.86524 with corrections 0.94205 1 observations identified as outliers and rejected Cycle 3 wR= 0.81413 Using Levenberg-Marquardt: 0.00000 New wR= 0.80851 There are 5 clusters with unrefined scales (size 34-55) Rint for refined data: 0.64518 with corrections 0.66939 Rint for all data: 0.86524 with corrections 0.88619 6 observations identified as outliers and rejected Cycle 4 wR= 0.65732 Using Levenberg-Marquardt: 0.00000 New wR= 0.64622 There are 5 clusters with unrefined scales (size 34-55) Rint for refined data: 0.64141 with corrections 0.64022 Rint for all data: 0.86524 with corrections 0.86368 6 observations identified as outliers and rejected Cycle 5 wR= 0.58244 Using Levenberg-Marquardt: 0.00000 New wR= 0.58168 There are 5 clusters with unrefined scales (size 34-55) Rint for refined data: 0.64016 with corrections 0.62693 Rint for all data: 0.86524 with corrections 0.85766 0 observations identified as outliers and rejected Final wR= 0.58168 Final frame scales: Min= 0.4758 Max= 1.0000 PROFFIT INFO: Inet (after scale3 abspack): min=787.4520 max=4057079.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=109.8787 max=54073.8945 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 2892 reflections read from tmp file 2263 reflections are rejected (2196 as outliers, 67 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 99 47 25 13 7 5 1 2 2 Initial Chi^2= 0.62839 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.82015 Current error model SIG(F2)^2 = 189.88*I_RAW + 0.00*I_BACK+(0.03642*)^2 Cycle 2, Chi^2= 1.00559 Current error model SIG(F2)^2 = 187.38*I_RAW + 0.00*I_BACK+(0.02160*)^2 Cycle 3, Chi^2= 1.00048 Current error model SIG(F2)^2 = 190.34*I_RAW + 0.00*I_BACK+(0.02095*)^2 Cycle 4, Chi^2= 0.99990 Current error model SIG(F2)^2 = 190.01*I_RAW + 0.00*I_BACK+(0.02112*)^2 Cycle 5, Chi^2= 1.00002 Current error model SIG(F2)^2 = 190.09*I_RAW + 0.00*I_BACK+(0.02108*)^2 Final Chi^2= 1.00002 Final error model SIG(F2)^2 = 190.09*I_RAW + 0.00*I_BACK+(0.02108*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4057080- 1079501 289 1743603.80 97.85 100.00 1078778- 628139 289 826567.67 47.42 100.00 626884- 247580 289 402806.44 46.37 100.00 247477- 157162 289 192319.50 33.07 100.00 157073- 122095 289 140291.87 22.74 100.00 121928- 90212 289 103333.12 17.01 100.00 90017- 68706 289 79608.85 13.70 100.00 68604- 5086 289 38120.00 9.55 94.81 5068- 2784 289 3692.86 3.47 59.86 2780- 787 291 2123.86 2.68 28.52 ------------------------------------------------------------------------------------ 4057080- 787 2892 353003.97 29.37 88.28 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 289 630685.46 61.76 96.89 1.32- 1.05 289 532727.81 43.52 94.46 1.05- 0.92 289 427616.85 34.92 91.00 0.92- 0.81 289 318984.32 27.62 85.12 0.81- 0.73 289 394415.37 28.20 90.66 0.73- 0.67 289 345436.60 26.36 88.24 0.67- 0.61 289 192014.50 18.00 82.01 0.61- 0.56 289 288339.63 20.55 84.08 0.56- 0.51 289 216408.36 17.82 84.08 0.51- 0.40 291 184576.42 15.05 86.25 ------------------------------------------------------------------------------------ 5.26- 0.40 2892 353003.97 29.37 88.28 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.32 289 630685.46 61.76 96.89 5.26- 1.05 578 581706.64 52.64 95.67 5.26- 0.92 867 530343.37 46.73 94.12 5.26- 0.81 1156 477503.61 41.95 91.87 5.26- 0.73 1445 460885.96 39.20 91.63 5.26- 0.67 1734 441644.40 37.06 91.06 5.26- 0.61 2023 405982.99 34.34 89.77 5.26- 0.56 2312 391277.57 32.62 89.06 5.26- 0.51 2601 371847.66 30.97 88.50 5.26- 0.40 2892 353003.97 29.37 88.28 ------------------------------------------------------------------------------------ 5.26- 0.40 2892 353003.97 29.37 88.28 Scale applied to data: s=0.246482 (maximum obs:4057079.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.858; Rsigma 0.023: data 2892 -> merged 316 With outlier rejection... Rint 0.815; Rsigma 0.023: data 2779 -> merged 316 Rejected total: 113, method kkm 98, method Blessing 15 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404276, 5.271121 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 13.67 100.00 205 1.46 - 1.12 15 15 20.73 100.00 311 1.08 - 0.96 15 15 17.53 100.00 263 0.96 - 0.86 15 15 16.00 100.00 240 0.86 - 0.79 15 15 14.07 100.00 211 0.79 - 0.73 15 15 12.20 100.00 183 0.73 - 0.69 15 15 11.40 100.00 171 0.69 - 0.65 15 15 11.47 100.00 172 0.65 - 0.63 15 15 7.67 100.00 115 0.63 - 0.60 21 21 8.38 100.00 176 --------------------------------------------------------------- 5.92 - 0.60 156 156 13.12 100.00 2047 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:25:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918020 5.914497 5.914344 60.0461 90.0904 60.0401 2779 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1393 1448 1395 1387 2118 1868 1849 2779 N (int>3sigma) = 0 1206 1448 1208 1258 1931 1661 1622 2452 Mean intensity = 0.0 80.6 35.2 80.2 80.7 64.9 87.7 84.5 85.8 Mean int/sigma = 0.0 29.4 24.6 28.9 28.5 27.6 29.7 28.9 29.3 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.915 90.06 119.94 119.95 Niggli form: a.a = 34.979 b.b = 34.981 c.c = 34.982 b.c = -0.036 a.c = -17.458 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.091 CUBIC F-lattice R(int) = 0.113 [ 2624] Vol = 585.8 Cell: 8.369 8.373 8.360 90.04 90.00 90.01 Volume: 585.83 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.078 RHOMBOHEDRAL R-lattice R(int) = 0.113 [ 2346] Vol = 439.4 Cell: 5.919 5.914 14.497 90.04 90.04 120.02 Volume: 439.37 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.078 RHOMBOHEDRAL R-lattice R(int) = 0.107 [ 747] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.497 90.04 90.04 120.02 Volume: 439.37 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.015 TETRAGONAL I-lattice R(int) = 0.107 [ 2380] Vol = 292.9 Cell: 5.920 5.919 8.360 89.98 89.97 89.97 Volume: 292.91 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.045 TETRAGONAL I-lattice R(int) = 0.107 [ 2380] Vol = 292.9 Cell: 5.919 5.920 8.360 90.03 90.02 89.97 Volume: 292.91 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.104 [ 2327] Vol = 292.9 Cell: 5.919 5.920 8.360 89.97 89.98 89.97 Volume: 292.91 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.039 ORTHORHOMBIC I-lattice R(int) = 0.103 [ 2326] Vol = 292.9 Cell: 5.914 8.369 5.918 89.99 89.91 89.99 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.020 MONOCLINIC I-lattice R(int) = 0.101 [ 1989] Vol = 292.9 Cell: 5.920 5.919 8.360 90.02 90.03 89.97 Volume: 292.91 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.066 MONOCLINIC I-lattice R(int) = 0.100 [ 1989] Vol = 292.9 Cell: 5.914 5.918 8.369 90.01 90.01 89.91 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.008 MONOCLINIC I-lattice R(int) = 0.100 [ 2011] Vol = 292.9 Cell: 5.914 8.369 5.918 89.99 90.09 90.01 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.039 MONOCLINIC I-lattice R(int) = 0.098 [ 1989] Vol = 292.9 Cell: 5.918 5.914 8.369 89.99 90.01 90.09 Volume: 292.91 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC C-lattice R(int) = 0.103 [ 1998] Vol = 292.9 Cell: 10.249 5.914 5.915 90.06 125.21 89.95 Volume: 292.91 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 1404] Vol = 146.5 Cell: 5.914 5.914 5.915 90.06 119.94 119.95 Volume: 146.46 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1448 0 1879 1862 2779 N (int>3sigma) = 0 0 0 0 1448 0 1669 1649 2452 Mean intensity = 0.0 0.0 0.0 0.0 35.2 0.0 85.3 86.2 85.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.6 0.0 28.9 29.5 29.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.164 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 30 30 202 635 N I>3s 27 27 126 635 1.0 1.0 0.8 41.7 6.8 6.8 3.8 30.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.113 2441 Fd-3m 1 1 227 C N N N N 37 2284 0.113 2479 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368662 8.373343 8.360142 90.0356 89.9994 90.0126 ZERR 1.00 0.003541 0.001642 0.000283 0.0012 0.0119 0.0016 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 2513091- 624609 407 387 31 12.5 927924.95 54.43 0.679 0.625 622445- 470466 352 349 31 11.3 543545.76 41.45 0.944 0.869 470433- 379490 355 349 31 11.3 408645.19 37.46 0.951 0.964 378838- 286610 319 311 31 10.0 315747.29 28.68 0.919 1.014 285764- 225130 301 289 31 9.3 231732.81 21.65 1.017 1.196 223270- 155093 330 308 31 9.9 167379.99 22.08 0.767 0.951 152273- 100798 257 242 31 7.8 102859.44 17.97 0.543 0.498 99693- 79687 208 198 31 6.4 80471.71 14.39 0.499 0.321 79380- 55044 203 196 31 6.3 65622.28 11.86 0.574 0.488 54345- 1907 160 150 37 4.1 38129.87 8.01 0.632 0.573 ------------------------------------------------------------------------------------------- 2513091- 1907 2892 2779 316 8.8 348164.68 29.26 0.815 0.807 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 559 541 31 17.5 598197.94 53.76 0.812 0.890 0.013 1.05-0.83 520 511 32 16.0 392249.52 32.47 0.917 1.073 0.020 0.82-0.72 407 396 31 12.8 330133.78 25.86 0.781 0.862 0.025 0.72-0.65 370 361 33 10.9 280253.41 23.23 0.892 0.948 0.027 0.64-0.60 274 261 31 8.4 276143.00 20.51 0.840 0.935 0.030 0.59-0.56 243 230 35 6.6 189560.80 16.69 0.662 0.649 0.037 0.55-0.52 190 182 31 5.9 255804.86 19.30 0.739 0.752 0.034 0.51-0.49 150 139 32 4.3 162384.68 14.75 0.646 0.557 0.041 0.49-0.45 108 97 32 3.0 174876.93 14.53 0.460 0.308 0.043 0.45-0.40 71 61 28 2.2 160939.06 13.73 0.340 0.241 0.047 ------------------------------------------------------------------------------------------------------ inf-0.40 2892 2779 316 8.8 348164.68 29.26 0.815 0.807 0.023 inf-0.60 2105 2047 156 13.1 402602.33 33.80 0.846 0.938 0.020 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 541 31 31 100.0 17.5 598197.94 270.03 0.812 0.004 1.05-0.83 511 32 32 100.0 16.0 392249.52 166.17 0.917 0.007 0.82-0.72 396 31 31 100.0 12.8 330133.78 117.06 0.781 0.009 0.72-0.65 361 33 33 100.0 10.9 280253.41 98.58 0.892 0.012 0.64-0.60 261 31 31 100.0 8.4 276143.00 77.79 0.840 0.014 0.59-0.56 230 38 35 92.1 6.6 189560.80 54.86 0.662 0.019 0.55-0.52 182 37 31 83.8 5.9 255804.86 58.69 0.739 0.017 0.51-0.49 139 44 32 72.7 4.3 162384.68 37.02 0.646 0.024 0.49-0.45 97 61 32 52.5 3.0 174876.93 29.94 0.460 0.027 0.45-0.40 61 125 28 22.4 2.2 160939.06 22.65 0.340 0.032 -------------------------------------------------------------------------------------------- inf-0.40 2779 463 316 68.3 8.8 348164.68 131.70 0.815 0.013 inf-0.60 2047 156 156 100.0 13.1 402602.33 162.00 0.846 0.008 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: 0.015561 -0.079444 -0.025025 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029172 0.072513 ( 0.000007 0.000007 0.000006 ) -0.076547 -0.003634 -0.036247 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007184 0.000002 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007176 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000004 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.015561 -0.079444 -0.025025 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029172 0.072513 ( 0.000007 0.000007 0.000006 ) -0.076547 -0.003634 -0.036247 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3687(5) 8.3734(7) 8.3602(6) 90.035(6) 89.999(6) 90.013(6) V = 585.84(7) unit cell: 8.36745(18) 8.36745(18) 8.36745(18) 90.0 90.0 90.0 V = 585.84(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.778) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.778) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.778) Run 5 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.778) PROFFIT INFO: signal sum: min=235.0000 max=20919086.0000 PROFFIT INFO: signal sum lp corr: min=473.0593 max=2975269.4472 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=756.8949 max=4760431.5000 PROFFIT INFO: sig(Inet): min=121.7004 max=47816.8594 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.32 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 60 278 608 1184 1332 2354 3862 5302 5784 Percent 0.0 0.0 1.0 4.8 10.5 20.5 23.0 40.7 66.8 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 2892 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 2892 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4760432- 1137875 289 1878248.64 121.87 100.00 1137848- 636838 289 865395.21 103.65 100.00 635920- 269029 289 421491.59 95.68 100.00 268714- 172101 289 205000.67 70.28 100.00 172040- 121576 289 146923.42 51.14 100.00 121562- 94982 289 107414.55 36.40 100.00 94870- 67683 289 82425.88 29.79 100.00 67570- 5611 289 37511.33 19.03 100.00 5597- 2977 289 3964.19 5.37 96.89 2972- 757 291 2139.86 3.72 55.33 ------------------------------------------------------------------------------------ 4760432- 757 2892 374793.64 53.66 95.19 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 289 739342.21 94.31 100.00 1.41- 1.12 289 659601.20 63.47 99.31 1.12- 0.96 289 455090.86 68.97 97.58 0.96- 0.88 289 365073.98 60.74 95.16 0.88- 0.81 289 462355.37 69.43 99.31 0.81- 0.73 289 244187.09 40.59 96.54 0.73- 0.71 289 176730.77 33.62 85.47 0.70- 0.65 289 327668.06 49.01 95.85 0.65- 0.62 289 160399.66 28.26 87.89 0.62- 0.58 291 158980.75 28.39 94.85 ------------------------------------------------------------------------------------ 4.82- 0.58 2892 374793.64 53.66 95.19 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:25:12 2018 Sorting 2892 observations 85 unique observations with > 7.00 F2/sig(F2) 2892 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 73 494 Total number of frames 494 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 2892 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 12 85 Total number of frames 85 2323 observations > 7.00 F2/sig(F2) 2323 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 12 85 Total number of frames 85 Removing 'redundancy=1' reflections Average redundancy: 24.9 (Out of 2323 removed 3 = 2320, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2320 observations in 5 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 12 85 Total number of frames 85 93 unique data precomputed (should be 93) 93 unique data with 2320 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.9 (Out of 2320 removed 0 = 2320, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2320 observations RMS deviation of equivalent data = 0.26140 Rint = 0.17907 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17060, wR= 0.26963 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13126, wR= 0.17757, Acormin=0.623, Acormax=1.404, Acor_av=0.971 F test: Probability=1.000, F= 1.685 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11668, wR= 0.14677, Acormin=0.510, Acormax=1.499, Acor_av=0.882 F test: Probability=1.000, F= 1.264 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10534, wR= 0.14603, Acormin=0.585, Acormax=1.551, Acor_av=0.935 F test: Probability=1.000, F= 1.224 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08946, wR= 0.11957, Acormin=0.470, Acormax=1.565, Acor_av=0.851 F test: Probability=1.000, F= 1.385 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07663, wR= 0.10771, Acormin=0.398, Acormax=1.588, Acor_av=0.849 F test: Probability=1.000, F= 1.359 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09748, wR= 0.13794, Acormin=0.621, Acormax=1.590, Acor_av=0.945 F test: Probability=0.000, F= 0.617 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08246, wR= 0.11382, Acormin=0.455, Acormax=1.596, Acor_av=0.857 F test: Probability=0.000, F= 0.861 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07232, wR= 0.10346, Acormin=0.392, Acormax=1.585, Acor_av=0.854 F test: Probability=0.995, F= 1.116 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07202, wR= 0.09931, Acormin=0.290, Acormax=1.332, Acor_av=0.725 F test: Probability=0.531, F= 1.003 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09402, wR= 0.13337, Acormin=0.544, Acormax=1.599, Acor_av=0.917 F test: Probability=0.000, F= 0.590 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08253, wR= 0.11168, Acormin=0.411, Acormax=1.480, Acor_av=0.773 F test: Probability=0.000, F= 0.764 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07681, wR= 0.10506, Acormin=0.107, Acormax=0.413, Acor_av=0.222 F test: Probability=0.000, F= 0.880 Trying model 13 (ne=8, no=5)... Results: Rint= 0.06962, wR= 0.09534, Acormin=0.118, Acormax=0.473, Acor_av=0.255 F test: Probability=0.930, F= 1.065 Trying model 14 (ne=8, no=7)... Results: Rint= 0.05865, wR= 0.08388, Acormin=0.156, Acormax=0.556, Acor_av=0.284 F test: Probability=1.000, F= 1.491 Final absorption model (ne=6, no=3): Rint= 0.07232, Acormin=0.392, Acormax=1.585, Acor_av=0.854 Combined refinement in use Rint: 0.17919 There are 85 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 121 pars with 7381 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26140 Using Levenberg-Marquardt: 0.00010 New wR= 0.06301 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17907 with corrections 0.05075 Rint for all data: 0.17919 with corrections 0.05096 0 observations identified as outliers and rejected Cycle 2 wR= 0.06301 Using Levenberg-Marquardt: 0.00001 New wR= 0.05721 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17907 with corrections 0.04563 Rint for all data: 0.17919 with corrections 0.04585 0 observations identified as outliers and rejected Cycle 3 wR= 0.05721 Using Levenberg-Marquardt: 0.00000 New wR= 0.05621 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17907 with corrections 0.04478 Rint for all data: 0.17919 with corrections 0.04499 0 observations identified as outliers and rejected Cycle 4 wR= 0.05621 Using Levenberg-Marquardt: 0.00000 New wR= 0.05572 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17907 with corrections 0.04441 Rint for all data: 0.17919 with corrections 0.04462 0 observations identified as outliers and rejected Cycle 5 wR= 0.05572 Using Levenberg-Marquardt: 0.00000 New wR= 0.05544 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17907 with corrections 0.04420 Rint for all data: 0.17919 with corrections 0.04441 0 observations identified as outliers and rejected Final wR= 0.05544 Final frame scales: Min= 0.7630 Max= 1.3313 Final absorption correction factors: Amin= 0.4898 Amax= 1.3920 PROFFIT INFO: Inet (after scale3 abspack): min=796.2912 max=4886219.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=112.5066 max=53207.4961 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 2892 reflections read from tmp file 567 reflections are rejected (566 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 6 1 1 3 2 6 3 84 Initial Chi^2= 0.35911 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.83145 Current error model SIG(F2)^2 = 125.64*I_RAW + 0.00*I_BACK+(0.02221*)^2 Cycle 2, Chi^2= 1.00026 Current error model SIG(F2)^2 = 109.21*I_RAW + 0.00*I_BACK+(0.01926*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 108.59*I_RAW + 0.00*I_BACK+(0.01940*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 108.69*I_RAW + 0.00*I_BACK+(0.01938*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 108.69*I_RAW + 0.00*I_BACK+(0.01938*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4886219- 1108069 289 1776528.59 47.77 100.00 1107791- 621039 289 822627.53 39.90 100.00 619990- 259605 289 408124.79 38.30 100.00 259591- 157131 289 194308.11 33.29 100.00 157031- 126838 289 141517.47 26.85 100.00 126753- 88674 289 103591.88 20.68 100.00 88637- 68956 289 79274.83 17.79 100.00 68839- 4905 289 39384.49 12.50 100.00 4876- 2758 289 3633.82 4.81 97.92 2757- 796 291 2161.13 3.95 80.41 ------------------------------------------------------------------------------------ 4886219- 796 2892 356869.79 24.57 97.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 289 746005.17 38.98 100.00 1.41- 1.12 289 636731.26 30.79 99.31 1.12- 0.96 289 416528.63 28.87 98.96 0.96- 0.88 289 343917.42 25.28 98.27 0.88- 0.81 289 436967.91 28.87 99.65 0.81- 0.73 289 225833.93 19.60 97.92 0.73- 0.71 289 164470.49 17.83 92.39 0.70- 0.65 289 304511.68 23.95 98.96 0.65- 0.62 289 148399.08 15.64 94.46 0.62- 0.58 291 146786.20 15.96 98.28 ------------------------------------------------------------------------------------ 4.82- 0.58 2892 356869.79 24.57 97.82 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 289 746005.17 38.98 100.00 4.82- 1.12 578 691368.21 34.88 99.65 4.82- 0.96 867 599755.02 32.88 99.42 4.82- 0.88 1156 535795.62 30.98 99.13 4.82- 0.81 1445 516030.08 30.56 99.24 4.82- 0.73 1734 467664.05 28.73 99.02 4.82- 0.71 2023 424350.69 27.17 98.07 4.82- 0.65 2312 409370.81 26.77 98.18 4.82- 0.62 2601 380373.95 25.53 97.77 4.82- 0.58 2892 356869.79 24.57 97.82 ------------------------------------------------------------------------------------ 4.82- 0.58 2892 356869.79 24.57 97.82 Scale applied to data: s=0.204657 (maximum obs:4886219.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.044; Rsigma 0.026: data 2892 -> merged 110 With outlier rejection... Rint 0.043; Rsigma 0.026: data 2875 -> merged 110 Rejected total: 17, method kkm 16, method Blessing 1 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585839, 4.830951 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 17.10 100.00 171 1.61 - 1.21 10 10 26.20 100.00 262 1.17 - 1.01 10 10 34.20 100.00 342 0.99 - 0.89 10 10 33.60 100.00 336 0.88 - 0.81 10 10 32.30 100.00 323 0.81 - 0.74 10 10 27.70 100.00 277 0.73 - 0.71 10 10 30.60 100.00 306 0.70 - 0.66 10 10 25.80 100.00 258 0.66 - 0.64 10 10 23.20 100.00 232 0.63 - 0.60 10 10 22.80 100.00 228 --------------------------------------------------------------- 5.92 - 0.60 100 100 27.35 100.00 2735 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:25:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.918020 5.914497 5.914344 60.0461 90.0904 60.0401 2779 Reflections read from file xs1714a.hkl; mean (I/sigma) = 29.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1393 1448 1395 1387 2118 1868 1849 2779 N (int>3sigma) = 0 1206 1448 1208 1258 1931 1661 1622 2452 Mean intensity = 0.0 80.6 35.2 80.2 80.7 64.9 87.7 84.5 85.8 Mean int/sigma = 0.0 29.4 24.6 28.9 28.5 27.6 29.7 28.9 29.3 Lattice type: P chosen Volume: 146.46 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.915 90.06 119.94 119.95 Niggli form: a.a = 34.979 b.b = 34.981 c.c = 34.982 b.c = -0.036 a.c = -17.458 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.091 CUBIC F-lattice R(int) = 0.113 [ 2624] Vol = 585.8 Cell: 8.369 8.373 8.360 90.04 90.00 90.01 Volume: 585.83 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.078 RHOMBOHEDRAL R-lattice R(int) = 0.113 [ 2346] Vol = 439.4 Cell: 5.919 5.914 14.497 90.04 90.04 120.02 Volume: 439.37 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.078 RHOMBOHEDRAL R-lattice R(int) = 0.107 [ 747] Vol = 439.4 Trigonal Cell: 5.919 5.914 14.497 90.04 90.04 120.02 Volume: 439.37 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.015 TETRAGONAL I-lattice R(int) = 0.107 [ 2380] Vol = 292.9 Cell: 5.920 5.919 8.360 89.98 89.97 89.97 Volume: 292.91 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.045 TETRAGONAL I-lattice R(int) = 0.107 [ 2380] Vol = 292.9 Cell: 5.919 5.920 8.360 90.03 90.02 89.97 Volume: 292.91 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.020 ORTHORHOMBIC I-lattice R(int) = 0.104 [ 2327] Vol = 292.9 Cell: 5.919 5.920 8.360 89.97 89.98 89.97 Volume: 292.91 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.039 ORTHORHOMBIC I-lattice R(int) = 0.103 [ 2326] Vol = 292.9 Cell: 5.914 8.369 5.918 89.99 89.91 89.99 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.020 MONOCLINIC I-lattice R(int) = 0.101 [ 1989] Vol = 292.9 Cell: 5.920 5.919 8.360 90.02 90.03 89.97 Volume: 292.91 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.066 MONOCLINIC I-lattice R(int) = 0.100 [ 1989] Vol = 292.9 Cell: 5.914 5.918 8.369 90.01 90.01 89.91 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.008 MONOCLINIC I-lattice R(int) = 0.100 [ 2011] Vol = 292.9 Cell: 5.914 8.369 5.918 89.99 90.09 90.01 Volume: 292.91 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.039 MONOCLINIC I-lattice R(int) = 0.098 [ 1989] Vol = 292.9 Cell: 5.918 5.914 8.369 89.99 90.01 90.09 Volume: 292.91 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.058 MONOCLINIC C-lattice R(int) = 0.103 [ 1998] Vol = 292.9 Cell: 10.249 5.914 5.915 90.06 125.21 89.95 Volume: 292.91 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.096 [ 1404] Vol = 146.5 Cell: 5.914 5.914 5.915 90.06 119.94 119.95 Volume: 146.46 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1448 0 1879 1862 2779 N (int>3sigma) = 0 0 0 0 1448 0 1669 1649 2452 Mean intensity = 0.0 0.0 0.0 0.0 35.2 0.0 85.3 86.2 85.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.6 0.0 28.9 29.5 29.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.164 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 30 30 202 635 N I>3s 27 27 126 635 1.0 1.0 0.8 41.7 6.8 6.8 3.8 30.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.113 2441 Fd-3m 1 1 227 C N N N N 37 2284 0.113 2479 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368662 8.373343 8.360142 90.0356 89.9994 90.0126 ZERR 1.00 0.003541 0.001642 0.000283 0.0012 0.0119 0.0016 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4034113- 527247 638 632 27 23.4 1229014.72 43.02 0.039 0.051 512237- 121903 860 859 27 31.8 217472.87 32.18 0.048 0.066 107813- 35799 714 710 27 26.3 79740.81 17.75 0.065 0.082 10363- 1845 680 674 29 23.2 3511.06 4.74 0.154 0.200 ------------------------------------------------------------------------------------------- 4034113- 1845 2892 2875 110 26.1 355662.23 24.57 0.043 0.055 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 722 716 27 26.5 633409.78 34.70 0.041 0.056 0.022 1.01-0.78 842 841 27 31.1 352114.39 24.95 0.030 0.037 0.026 0.78-0.65 817 812 29 28.0 232124.17 19.70 0.050 0.059 0.032 0.65-0.59 511 506 27 18.7 166787.53 17.39 0.076 0.086 0.039 ------------------------------------------------------------------------------------------------------ inf-0.59 2892 2875 110 26.1 355662.23 24.57 0.043 0.055 0.026 inf-0.60 2750 2733 99 27.6 368053.21 25.07 0.042 0.054 0.026 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 716 27 27 100.0 26.5 633409.78 201.83 0.041 0.006 1.01-0.78 841 27 27 100.0 31.1 352114.39 149.81 0.030 0.005 0.78-0.65 812 29 29 100.0 28.0 232124.17 109.65 0.050 0.007 0.65-0.59 506 27 27 100.0 18.7 166787.53 87.83 0.076 0.012 -------------------------------------------------------------------------------------------- inf-0.59 2875 110 110 100.0 26.1 355662.23 140.51 0.043 0.007 inf-0.60 2733 99 99 100.0 27.6 368053.21 144.17 0.042 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:31:59 2018) ID: 2932; threads 39; handles 877; mem 520084.00 (1237700.00)kB; time: 1w 5d 0h 37m 30s MEMORY INFO: Memory PF:0.0, Ph:231.0, V:1208.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:507.9,peak PF: 697.1, WS: 298.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:231.0, V:1210.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:509.7,peak PF: 697.1, WS: 300.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:31:59 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000011 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000012 0.000014 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) 5.91502 ( 0.00074 ) 5.91640 ( 0.00074 ) 5.92265 ( 0.00062 ) 60.05206 ( 0.01201 ) 89.98756 ( 0.00932 ) 60.01743 ( 0.01310 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:31:59 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000011 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000012 0.000014 0.000013 ) 0.109112 -0.153091 0.115835 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.021545 -0.014364 0.007206 ( 0.000003 0.000002 0.000002 ) -0.014364 0.028735 -0.014370 ( 0.000002 0.000004 0.000002 ) 0.007206 -0.014370 0.021570 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(7) 5.9164(7) 5.9227(6) 60.052(12) 89.988(9) 60.017(13) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 408 peaks identified as outliers and rejected 405 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 405 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 405 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 41 | 0.986 ( 0.139) | 1.248 ( 0.679) | 1.208 ( 0.948) | 1.32- 1.09 | 41 | 1.026 ( 0.082) | 1.097 ( 0.108) | 1.031 ( 0.412) | 1.09- 0.96 | 41 | 1.014 ( 0.092) | 1.142 ( 0.369) | 1.053 ( 0.432) | 0.96- 0.85 | 41 | 1.000 ( 0.089) | 1.047 ( 0.140) | 1.071 ( 0.398) | 0.85- 0.81 | 41 | 1.018 ( 0.080) | 1.057 ( 0.138) | 1.034 ( 0.259) | 0.81- 0.73 | 41 | 0.983 ( 0.062) | 1.040 ( 0.152) | 1.080 ( 0.379) | 0.73- 0.69 | 41 | 0.973 ( 0.056) | 0.940 ( 0.114) | 1.209 ( 0.582) | 0.69- 0.65 | 41 | 0.959 ( 0.042) | 0.898 ( 0.083) | 1.213 ( 0.446) | 0.65- 0.63 | 41 | 0.921 ( 0.026) | 0.853 ( 0.041) | 1.254 ( 0.473) | 0.63- 0.59 | 36 | 0.892 ( 0.034) | 0.828 ( 0.060) | 1.244 ( 0.474) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 405 | 0.978 ( 0.087) | 1.017 ( 0.294) | 1.138 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 483 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.146) | 1.119 ( 0.425) | 1.108 ( 0.576) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.274 ( 0.643) | 1.098 ( 0.630) | 1.12- 0.98 | 47 | 1.023 ( 0.100) | 1.063 ( 0.158) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.028 ( 0.093) | 1.030 ( 0.135) | 1.096 ( 0.435) | 0.89- 0.82 | 47 | 1.038 ( 0.085) | 1.008 ( 0.123) | 1.182 ( 0.495) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.170 ( 0.494) | 0.75- 0.71 | 47 | 1.026 ( 0.045) | 0.937 ( 0.113) | 1.293 ( 0.516) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.887 ( 0.071) | 1.263 ( 0.497) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.299 ( 0.514) | 0.63- 0.59 | 50 | 0.944 ( 0.055) | 0.814 ( 0.041) | 1.354 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 473 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.184 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 473 obs out of 473 (total:473,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088654 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010205 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116128 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 473 1 1 1 OTKP changes: 473 1 1 1 OTKP changes: 473 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068770 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 473 obs out of 473 (total:473,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068770 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 473 obs out of 473 (total:473,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 473 obs out of 473 (total:473,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.014 ( 0.108) | 1.028 ( 0.130) | 0.949 ( 0.328) | 0.97- 0.89 | 47 | 1.028 ( 0.089) | 1.029 ( 0.137) | 1.105 ( 0.406) | 0.88- 0.82 | 47 | 1.047 ( 0.080) | 1.020 ( 0.120) | 1.212 ( 0.510) | 0.82- 0.75 | 47 | 1.037 ( 0.080) | 0.987 ( 0.126) | 1.069 ( 0.407) | 0.75- 0.71 | 47 | 1.022 ( 0.044) | 0.934 ( 0.110) | 1.339 ( 0.543) | 0.71- 0.67 | 47 | 0.997 ( 0.043) | 0.885 ( 0.072) | 1.211 ( 0.465) | 0.67- 0.63 | 47 | 0.974 ( 0.047) | 0.841 ( 0.041) | 1.287 ( 0.499) | 0.63- 0.59 | 49 | 0.949 ( 0.045) | 0.812 ( 0.041) | 1.347 ( 0.519) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 472 | 1.014 ( 0.090) | 0.993 ( 0.294) | 1.174 ( 0.533) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb PROFFITPEAK info: 1139 peaks in the peak location table UB fit with 523 obs out of 550 (total:550,skipped:0) (95.09%) UB - matrix: -0.069499 0.031165 0.088917 ( 0.000043 0.000070 0.000062 ) -0.069000 -0.065444 -0.010175 ( 0.000031 0.000051 0.000045 ) 0.108929 -0.152990 0.116088 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021457 -0.014315 0.007168 ( 0.000013 0.000013 0.000012 ) -0.014315 0.028660 -0.014323 ( 0.000013 0.000026 0.000016 ) 0.007168 -0.014323 0.021486 ( 0.000012 0.000016 0.000020 ) unit cell: 5.930(3) 5.923(3) 5.926(3) 60.03(5) 90.05(4) 60.02(5) V = 147.23(11) UB fit with 523 obs out of 550 (total:550,skipped:0) (95.09%) UB - matrix: -0.069499 0.031165 0.088917 ( 0.000043 0.000070 0.000062 ) -0.069000 -0.065444 -0.010175 ( 0.000031 0.000051 0.000045 ) 0.108929 -0.152990 0.116088 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021457 -0.014315 0.007168 ( 0.000013 0.000013 0.000012 ) -0.014315 0.028660 -0.014323 ( 0.000013 0.000026 0.000016 ) 0.007168 -0.014323 0.021486 ( 0.000012 0.000016 0.000020 ) unit cell: 5.930(3) 5.923(3) 5.926(3) 60.03(5) 90.05(4) 60.02(5) V = 147.23(11) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 550 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 526 obs out of 550 (total:550,skipped:0) (95.64%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 451 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 448 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 448 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.48 | 45 | 0.999 ( 0.191) | 1.283 ( 0.753) | 1.137 ( 0.704) | 1.47- 1.17 | 45 | 1.014 ( 0.087) | 1.064 ( 0.193) | 0.971 ( 0.388) | 1.17- 0.98 | 45 | 1.007 ( 0.082) | 1.020 ( 0.115) | 0.971 ( 0.404) | 0.98- 0.92 | 45 | 0.998 ( 0.077) | 0.997 ( 0.120) | 1.059 ( 0.407) | 0.89- 0.82 | 45 | 1.013 ( 0.065) | 0.976 ( 0.102) | 1.258 ( 0.536) | 0.82- 0.75 | 45 | 0.990 ( 0.079) | 0.973 ( 0.124) | 1.109 ( 0.415) | 0.75- 0.71 | 45 | 0.972 ( 0.047) | 0.921 ( 0.064) | 1.238 ( 0.437) | 0.71- 0.67 | 45 | 0.948 ( 0.043) | 0.870 ( 0.063) | 1.252 ( 0.513) | 0.67- 0.62 | 45 | 0.912 ( 0.034) | 0.839 ( 0.045) | 1.384 ( 0.529) | 0.62- 0.59 | 43 | 0.885 ( 0.033) | 0.814 ( 0.038) | 1.452 ( 0.610) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 0.974 ( 0.096) | 0.976 ( 0.289) | 1.182 ( 0.527) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.069868 0.031444 0.088851 ( 0.000020 0.000034 0.000027 ) -0.068937 -0.065439 -0.010099 ( 0.000017 0.000028 0.000023 ) 0.109191 -0.152972 0.116370 ( 0.000018 0.000030 0.000024 ) M - matrix: 0.021557 -0.014389 0.007195 ( 0.000005 0.000005 0.000005 ) -0.014389 0.028672 -0.014347 ( 0.000005 0.000010 0.000006 ) 0.007195 -0.014347 0.021538 ( 0.000005 0.000006 0.000007 ) unit cell: 5.9241(14) 5.9300(14) 5.9191(13) 60.02(2) 89.980(19) 59.90(2) V = 146.89(5) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.069613 0.031297 0.088856 ( 0.000019 0.000032 0.000026 ) -0.068939 -0.065449 -0.010080 ( 0.000017 0.000028 0.000023 ) 0.109040 -0.153008 0.116186 ( 0.000014 0.000024 0.000019 ) M - matrix: 0.021488 -0.014351 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014351 0.028674 -0.014337 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014337 0.021496 ( 0.000004 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9302(14) 5.9268(14) 5.9256(13) 60.02(2) 90.013(19) 59.96(2) V = 147.19(5) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069613 0.031297 0.088856 ( 0.000019 0.000032 0.000026 ) -0.068939 -0.065449 -0.010080 ( 0.000017 0.000028 0.000023 ) 0.109040 -0.153008 0.116186 ( 0.000014 0.000024 0.000019 ) M - matrix: 0.021488 -0.014351 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014351 0.028674 -0.014337 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014337 0.021496 ( 0.000004 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9302(14) 5.9268(14) 5.9256(13) 60.02(2) 90.013(19) 59.96(2) V = 147.19(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 455 peaks identified as outliers and rejected 452 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 452 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 452 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 45 | 0.996 ( 0.196) | 1.198 ( 0.653) | 1.142 ( 0.733) | 1.48- 1.17 | 45 | 1.016 ( 0.088) | 1.087 ( 0.336) | 0.977 ( 0.385) | 1.17- 0.99 | 45 | 1.007 ( 0.081) | 1.044 ( 0.122) | 0.963 ( 0.386) | 0.99- 0.92 | 45 | 0.998 ( 0.081) | 1.001 ( 0.112) | 1.011 ( 0.408) | 0.92- 0.82 | 45 | 1.009 ( 0.070) | 0.966 ( 0.103) | 1.286 ( 0.515) | 0.82- 0.76 | 45 | 0.996 ( 0.078) | 0.976 ( 0.125) | 1.121 ( 0.441) | 0.76- 0.71 | 45 | 0.971 ( 0.051) | 0.930 ( 0.077) | 1.217 ( 0.451) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.879 ( 0.064) | 1.279 ( 0.537) | 0.67- 0.63 | 45 | 0.915 ( 0.035) | 0.844 ( 0.043) | 1.404 ( 0.536) | 0.63- 0.59 | 47 | 0.887 ( 0.034) | 0.813 ( 0.037) | 1.429 ( 0.608) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 452 | 0.974 ( 0.097) | 0.973 ( 0.269) | 1.184 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 225 | 1.115 ( 0.122) | 1.218 ( 0.427) | 1.170 ( 0.589) | 13.2-19.0 | 225 | 1.077 ( 0.053) | 1.130 ( 0.276) | 1.185 ( 0.517) | 19.0-23.1 | 225 | 1.064 ( 0.071) | 1.146 ( 0.399) | 1.184 ( 0.536) | 23.1-27.1 | 225 | 1.032 ( 0.076) | 1.064 ( 0.256) | 1.173 ( 0.558) | 27.2-30.8 | 225 | 1.009 ( 0.071) | 1.005 ( 0.235) | 1.183 ( 0.489) | 30.8-33.8 | 225 | 0.978 ( 0.079) | 0.940 ( 0.231) | 1.207 ( 0.515) | 33.8-36.9 | 225 | 0.960 ( 0.074) | 0.901 ( 0.106) | 1.179 ( 0.485) | 36.9-39.6 | 225 | 0.944 ( 0.085) | 0.871 ( 0.131) | 1.218 ( 0.552) | 39.6-42.7 | 225 | 0.921 ( 0.073) | 0.835 ( 0.078) | 1.207 ( 0.548) | 42.7-49.9 | 226 | 0.926 ( 0.086) | 0.810 ( 0.065) | 1.138 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2251 | 1.002 ( 0.103) | 0.992 ( 0.285) | 1.184 ( 0.528) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0024 b=1.00 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10984832 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:32:23 2018 PROFFITMAIN - Started at Tue Mar 27 15:32:23 2018 OTKP changes: 2251 2 4 5 OTKP changes: 2251 2 4 5 UB - matrix: -0.070074 0.031150 0.088955 ( 0.000011 0.000013 0.000012 ) -0.068745 -0.065897 -0.010384 ( 0.000010 0.000012 0.000011 ) 0.109189 -0.153089 0.116378 ( 0.000009 0.000010 0.000009 ) M - matrix: 0.021559 -0.014368 0.007188 ( 0.000003 0.000002 0.000002 ) -0.014368 0.028749 -0.014361 ( 0.000002 0.000004 0.000002 ) 0.007188 -0.014361 0.021565 ( 0.000002 0.000002 0.000003 ) UB fit with 2251 obs out of 2251 (total:2251,skipped:0) (100.00%) unit cell: 5.9155(7) 5.9120(7) 5.9127(6) 60.051(11) 90.041(9) 60.018(12) V = 146.32(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070073 0.030679 0.088931 ( 0.000028 0.000028 0.000016 ) -0.068224 -0.066129 -0.010546 ( 0.000025 0.000024 0.000014 ) 0.109089 -0.153071 0.116009 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021465 -0.014337 0.007143 ( 0.000007 0.000006 0.000004 ) -0.014337 0.028745 -0.014332 ( 0.000006 0.000008 0.000004 ) 0.007143 -0.014332 0.021478 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9284(14) 5.9142(14) 5.9248(11) 60.02(2) 89.980(17) 59.99(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109367 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109367 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109367 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) UB - matrix: -0.070406 0.031323 0.088620 ( 0.000025 0.000022 0.000027 ) -0.068589 -0.065974 -0.010269 ( 0.000031 0.000027 0.000033 ) 0.109002 -0.152698 0.116261 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021543 -0.014325 0.007138 ( 0.000007 0.000005 0.000005 ) -0.014325 0.028650 -0.014299 ( 0.000005 0.000006 0.000005 ) 0.007138 -0.014299 0.021476 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9148(16) 5.9212(16) 5.9235(13) 60.02(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 OTKP changes: 405 1 1 1 UB - matrix: -0.070380 0.031254 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068828 -0.065838 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109174 -0.153164 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014390 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014390 0.028771 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070380 0.031254 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068828 -0.065838 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109174 -0.153164 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014390 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014390 0.028771 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070380 0.031254 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068828 -0.065838 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109174 -0.153164 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014390 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014390 0.028771 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 405 obs out of 405 (total:405,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) UB - matrix: -0.070118 0.031473 0.088650 ( 0.000016 0.000025 0.000021 ) -0.068840 -0.065724 -0.010157 ( 0.000020 0.000031 0.000026 ) 0.108946 -0.152898 0.116187 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021525 -0.014340 0.007141 ( 0.000005 0.000005 0.000004 ) -0.014340 0.028688 -0.014307 ( 0.000005 0.000009 0.000005 ) 0.007141 -0.014307 0.021461 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9198(15) 5.9195(15) 5.9260(11) 60.02(2) 89.959(17) 59.98(3) V = 146.91(5) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 UB - matrix: -0.070176 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066050 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9141(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070176 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066050 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9141(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070176 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066050 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9141(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) UB - matrix: -0.069818 0.031400 0.088871 ( 0.000020 0.000033 0.000027 ) -0.068966 -0.065428 -0.010108 ( 0.000017 0.000028 0.000022 ) 0.109166 -0.153001 0.116341 ( 0.000018 0.000029 0.000024 ) M - matrix: 0.021548 -0.014382 0.007193 ( 0.000005 0.000005 0.000004 ) -0.014382 0.028676 -0.014348 ( 0.000005 0.000010 0.000006 ) 0.007193 -0.014348 0.021535 ( 0.000004 0.000006 0.000007 ) unit cell: 5.9243(14) 5.9289(14) 5.9199(13) 60.02(2) 89.986(19) 59.91(2) V = 146.90(5) OTKP changes: 452 1 1 1 OTKP changes: 452 1 1 1 OTKP changes: 452 1 1 1 UB - matrix: -0.069946 0.031440 0.088981 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069946 0.031440 0.088981 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.069946 0.031440 0.088981 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.069981 0.031128 0.088929 ( 0.000011 0.000013 0.000012 ) -0.068795 -0.065791 -0.010437 ( 0.000011 0.000014 0.000012 ) 0.109164 -0.153105 0.116431 ( 0.000008 0.000010 0.000009 ) M - matrix: 0.021547 -0.014366 0.007205 ( 0.000003 0.000002 0.000002 ) -0.014366 0.028739 -0.014371 ( 0.000002 0.000004 0.000002 ) 0.007205 -0.014371 0.021574 ( 0.000002 0.000002 0.000003 ) UB fit with 2251 obs out of 2251 (total:2251,skipped:0) (100.00%) unit cell: 5.9179(7) 5.9142(7) 5.9136(6) 60.046(12) 90.083(9) 60.035(13) V = 146.42(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 65 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof 3047 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:32:29 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) PROFFIT INFO: signal sum: min=235.0000 max=20917466.0000 PROFFIT INFO: signal sum lp corr: min=469.1951 max=2977048.4106 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=750.7121 max=4763277.5000 PROFFIT INFO: sig(Inet): min=120.4339 max=47821.4961 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 33 149 318 624 700 1246 2040 2795 3047 Percent 0.0 0.0 1.1 4.9 10.4 20.5 23.0 40.9 67.0 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4763278- 1126878 304 1857504.16 122.09 100.00 1120723- 632084 304 856456.38 102.98 100.00 631645- 267497 304 418560.97 94.92 100.00 267413- 170043 304 203629.39 70.39 100.00 170002- 120782 304 145593.02 51.27 100.00 120558- 94182 304 106661.93 36.29 100.00 94162- 67230 304 81545.53 29.59 100.00 67065- 5692 304 38005.19 19.24 100.00 5683- 2972 304 3973.94 5.40 97.04 2970- 751 311 2127.92 3.72 54.98 ------------------------------------------------------------------------------------ 4763278- 751 3047 370557.48 53.47 95.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 304 625641.72 86.37 99.34 1.41- 1.05 304 603777.27 69.32 97.70 1.05- 0.92 304 450381.13 61.40 98.36 0.92- 0.82 304 325283.46 51.60 94.08 0.82- 0.74 304 429754.80 57.72 96.05 0.74- 0.67 304 360735.39 55.89 96.38 0.67- 0.61 304 202950.05 37.59 93.75 0.61- 0.56 304 295315.57 45.00 92.11 0.56- 0.51 304 226846.24 37.94 90.46 0.51- 0.40 311 189068.25 32.38 92.93 ------------------------------------------------------------------------------------ 5.26- 0.40 3047 370557.48 53.47 95.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:32:29 2018 Sorting 3047 observations 295 unique observations with > 7.00 F2/sig(F2) 3047 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 98 519 Total number of frames 519 Maximum number of 295 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 3047 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 2446 observations > 7.00 F2/sig(F2) 2446 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 2446 removed 24 = 2422, unique = 284) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2422 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 284 unique data precomputed (should be 284) 284 unique data with 2422 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 2422 removed 0 = 2422, unique = 284) 284 unique data precomputed (should be 284) 284 unique data with 2422 observations RMS deviation of equivalent data = 0.73699 Rint = 0.69842 14 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.67905, wR= 3.49957 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68775, wR= 2.85647, Acormin=0.137, Acormax=1.981, Acor_av=0.839 F test: Probability=0.000, F= 0.973 Trying model 2 (ne=2, no=1)... Results: Rint= 0.73046, wR= 2.84976, Acormin=-0.166, Acormax=1.876, Acor_av=0.737 F test: Probability=0.000, F= 0.861 Trying model 3 (ne=4, no=0)... Results: Rint= 0.73163, wR= 2.44962, Acormin=-0.172, Acormax=2.319, Acor_av=0.699 F test: Probability=0.000, F= 0.856 Trying model 4 (ne=4, no=1)... Results: Rint= 0.78164, wR= 2.39135, Acormin=-0.523, Acormax=1.923, Acor_av=0.599 F test: Probability=0.000, F= 0.749 Trying model 5 (ne=4, no=3)... Results: Rint= 0.78857, wR= 2.47342, Acormin=-0.727, Acormax=1.960, Acor_av=0.537 F test: Probability=0.000, F= 0.733 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75195, wR= 2.39674, Acormin=-0.324, Acormax=2.621, Acor_av=0.632 F test: Probability=0.000, F= 0.805 Trying model 7 (ne=6, no=1)... Results: Rint= 0.79913, wR= 2.39097, Acormin=-0.561, Acormax=2.252, Acor_av=0.523 F test: Probability=0.000, F= 0.712 Trying model 8 (ne=6, no=3)... Results: Rint= 0.81526, wR= 2.43358, Acormin=-0.994, Acormax=2.099, Acor_av=0.461 F test: Probability=0.000, F= 0.682 Trying model 9 (ne=6, no=5)... Results: Rint= 0.83940, wR= 2.47636, Acormin=-1.103, Acormax=2.237, Acor_av=0.380 F test: Probability=0.000, F= 0.640 Trying model 10 (ne=8, no=0)... Results: Rint= 0.82610, wR= 2.16297, Acormin=-0.711, Acormax=2.176, Acor_av=0.452 F test: Probability=0.000, F= 0.662 Trying model 11 (ne=8, no=1)... Results: Rint= 0.89935, wR= 1.82701, Acormin=-0.943, Acormax=1.488, Acor_av=0.250 F test: Probability=0.000, F= 0.557 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98809, wR= 1.55042, Acormin=-0.047, Acormax=0.068, Acor_av=0.001 F test: Probability=0.000, F= 0.460 Trying model 13 (ne=8, no=5)... Results: Rint= 0.98958, wR= 1.58018, Acormin=-0.054, Acormax=0.068, Acor_av=0.002 F test: Probability=0.000, F= 0.456 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00377, wR= 1.66901, Acormin=-0.050, Acormax=0.065, Acor_av=0.001 F test: Probability=0.000, F= 0.440 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86663 There are 263 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 267 pars with 35778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.73699 Using Levenberg-Marquardt: 0.00010 New wR= 0.71484 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.69842 with corrections 0.67664 Rint for all data: 0.86663 with corrections 0.85122 15 observations identified as outliers and rejected Cycle 2 wR= 0.68949 Using Levenberg-Marquardt: 0.00001 New wR= 0.68725 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67803 with corrections 0.66084 Rint for all data: 0.86663 with corrections 0.85701 11 observations identified as outliers and rejected Cycle 3 wR= 0.66888 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.66481 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66812 with corrections 0.65067 Rint for all data: 0.86663 with corrections 0.85654 10 observations identified as outliers and rejected Cycle 4 wR= 0.64222 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64082 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66370 with corrections 0.66138 Rint for all data: 0.86663 with corrections 0.86587 3 observations identified as outliers and rejected Cycle 5 wR= 0.63787 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.63105 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66142 with corrections 0.66101 Rint for all data: 0.86663 with corrections 0.86556 5 observations identified as outliers and rejected Final wR= 0.63105 Final frame scales: Min= 1.0000 Max= 7.1167 Final absorption correction factors: Amin= 0.2269 Amax= 1.7578 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 263 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 267 pars with 35778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.84586 Using Levenberg-Marquardt: 0.00010 New wR= 0.84928 Using Levenberg-Marquardt: 0.00100 New wR= 0.81216 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65894 with corrections 1.43590 Rint for all data: 0.86663 with corrections 1.48628 2 observations identified as outliers and rejected Cycle 2 wR= 0.80266 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.68862 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65840 with corrections 1.33925 Rint for all data: 0.86663 with corrections 1.37782 3 observations identified as outliers and rejected Cycle 3 wR= 0.68361 Using Levenberg-Marquardt: 0.01000 New wR= 0.63131 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65789 with corrections 1.03746 Rint for all data: 0.86663 with corrections 1.13831 3 observations identified as outliers and rejected Cycle 4 wR= 0.62941 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.62122 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65722 with corrections 0.73019 Rint for all data: 0.86663 with corrections 0.90823 1 observations identified as outliers and rejected Cycle 5 wR= 0.62040 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.61523 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65708 with corrections 0.68879 Rint for all data: 0.86663 with corrections 0.88277 2 observations identified as outliers and rejected Final wR= 0.61523 Final frame scales: Min= 0.4337 Max= 5.7749 Final absorption correction factors: Amin= 0.1006 Amax= 1.7992 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 251 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 255 pars with 32640 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.75042 Using Levenberg-Marquardt: 0.00010 New wR= 0.63429 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65624 with corrections 0.66046 Rint for all data: 0.86663 with corrections 0.87026 8 observations identified as outliers and rejected Cycle 2 wR= 0.59786 Using Levenberg-Marquardt: 0.00001 New wR= 0.58191 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65379 with corrections 0.63023 Rint for all data: 0.86663 with corrections 0.85376 6 observations identified as outliers and rejected Cycle 3 wR= 0.56454 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.56441 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65223 with corrections 0.62820 Rint for all data: 0.86663 with corrections 0.85505 Final wR= 0.56441 Final frame scales: Min= 0.8327 Max= 2.7459 Final absorption correction factors: Amin= 0.3320 Amax= 1.4480 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=661.7578 max=5908888.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=120.8692 max=65805.7500 PROFFIT INFO: 14 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 3033 reflections read from tmp file 2267 reflections are rejected (2204 as outliers, 63 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 79 64 31 23 10 9 2 3 1 Initial Chi^2= 0.66620 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93157 Current error model SIG(F2)^2 = 298.53*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 278.10*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 278.10*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5908888- 1093395 303 1842302.43 87.77 100.00 1088885- 572764 303 804799.28 42.96 100.00 570347- 255817 303 391342.78 38.84 100.00 255582- 159095 303 200300.00 29.81 100.00 158616- 120821 303 138872.68 20.10 100.00 120589- 87337 303 103327.70 15.11 100.00 87304- 61247 303 73140.64 11.81 100.00 61200- 5510 303 35830.53 8.58 92.41 5494- 2605 303 3620.45 3.01 32.01 2603- 662 306 2016.66 2.43 16.34 ------------------------------------------------------------------------------------ 5908888- 662 3033 359201.67 26.02 84.01 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 303 736052.33 57.14 95.05 1.41- 1.05 303 592515.84 39.54 93.07 1.05- 0.92 303 447605.39 30.74 89.11 0.92- 0.82 303 315722.75 22.81 79.54 0.82- 0.74 303 422163.45 25.83 86.47 0.74- 0.67 303 331386.26 22.62 84.49 0.67- 0.61 303 177933.32 14.99 77.89 0.61- 0.56 303 249738.68 18.04 78.22 0.56- 0.51 303 184311.86 15.33 78.55 0.51- 0.40 306 136788.91 13.28 77.78 ------------------------------------------------------------------------------------ 5.26- 0.40 3033 359201.67 26.02 84.01 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 303 736052.33 57.14 95.05 5.26- 1.05 606 664284.09 48.34 94.06 5.26- 0.92 909 592057.85 42.47 92.41 5.26- 0.82 1212 522974.08 37.56 89.19 5.26- 0.74 1515 502811.95 35.21 88.65 5.26- 0.67 1818 474241.00 33.11 87.95 5.26- 0.61 2121 431911.33 30.52 86.52 5.26- 0.56 2424 409139.75 28.96 85.48 5.26- 0.51 2727 384158.87 27.45 84.71 5.26- 0.40 3033 359201.67 26.02 84.01 ------------------------------------------------------------------------------------ 5.26- 0.40 3033 359201.67 26.02 84.01 Scale applied to data: s=0.169236 (maximum obs:5908888.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.852; Rsigma 0.025: data 3033 -> merged 319 With outlier rejection... Rint 0.798; Rsigma 0.025: data 2906 -> merged 319 Rejected total: 127, method kkm 113, method Blessing 14 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404247, 5.270732 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 14.67 100.00 220 1.46 - 1.12 15 15 21.80 100.00 327 1.08 - 0.96 15 15 18.13 100.00 272 0.96 - 0.86 15 15 16.67 100.00 250 0.86 - 0.79 15 15 14.53 100.00 218 0.79 - 0.73 15 15 12.73 100.00 191 0.73 - 0.69 15 15 11.80 100.00 177 0.69 - 0.65 15 15 12.13 100.00 182 0.65 - 0.63 15 15 7.87 100.00 118 0.63 - 0.60 21 21 8.62 100.00 181 --------------------------------------------------------------- 5.92 - 0.60 156 156 13.69 100.00 2136 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:32:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917898 5.914164 5.913554 60.0465 90.0831 60.0348 2905 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.61 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1461 1523 1454 1463 2219 1954 1924 2905 N (int>3sigma) = 0 1199 1523 1192 1218 1957 1649 1614 2435 Mean intensity = 0.0 54.2 24.4 54.2 55.4 44.0 60.1 57.8 58.4 Mean int/sigma = 0.0 24.8 21.4 24.5 24.7 23.5 26.1 25.6 25.6 Lattice type: P chosen Volume: 146.42 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.914 90.06 119.94 119.95 Niggli form: a.a = 34.970 b.b = 34.977 c.c = 34.980 b.c = -0.034 a.c = -17.457 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.089 CUBIC F-lattice R(int) = 0.176 [ 2749] Vol = 585.7 Cell: 8.368 8.372 8.360 90.04 90.00 90.01 Volume: 585.70 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 2470] Vol = 439.3 Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.27 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.170 [ 788] Vol = 439.3 Trigonal Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.27 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.018 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.8 Cell: 5.919 5.918 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.049 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.8 Cell: 5.918 5.919 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 2452] Vol = 292.8 Cell: 5.918 5.919 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.148 [ 2451] Vol = 292.8 Cell: 5.914 8.368 5.918 89.99 89.92 89.99 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.138 [ 2113] Vol = 292.8 Cell: 5.919 5.918 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.060 MONOCLINIC I-lattice R(int) = 0.139 [ 2114] Vol = 292.8 Cell: 5.914 5.918 8.368 90.01 90.01 89.92 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.007 MONOCLINIC I-lattice R(int) = 0.138 [ 2135] Vol = 292.8 Cell: 5.914 8.368 5.918 89.99 90.08 90.01 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.036 MONOCLINIC I-lattice R(int) = 0.131 [ 2112] Vol = 292.8 Cell: 5.918 5.914 8.368 89.99 90.01 90.08 Volume: 292.85 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.157 [ 2120] Vol = 292.8 Cell: 10.247 5.914 5.914 90.06 125.21 89.95 Volume: 292.85 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.117 [ 1528] Vol = 146.4 Cell: 5.914 5.914 5.914 90.06 119.94 119.95 Volume: 146.42 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1523 0 1956 1946 2905 N (int>3sigma) = 0 0 0 0 1523 0 1647 1647 2435 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 57.8 58.4 58.4 Mean int/sigma = 0.0 0.0 0.0 0.0 21.4 0.0 25.5 25.7 25.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.143 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 217 661 N I>3s 28 28 102 661 0.8 0.8 0.6 29.1 6.3 6.3 3.5 26.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.176 2552 Fd-3m 1 1 227 C N N N N 37 2284 0.176 2590 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368104 8.372165 8.360031 90.0421 89.9976 90.0109 ZERR 1.00 0.003434 0.001602 0.000272 0.0011 0.0115 0.0014 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3074982- 584564 527 503 31 16.2 888960.65 53.43 0.701 0.684 584465- 444832 376 369 31 11.9 508326.92 32.03 0.944 0.873 420780- 334250 333 329 31 10.6 376582.05 28.85 0.902 0.875 332980- 271806 345 335 31 10.8 287186.11 22.98 0.936 1.008 268043- 202197 280 260 31 8.4 190431.13 16.34 0.922 0.972 201663- 151754 327 308 31 9.9 160282.98 18.66 0.741 0.941 148977- 91401 294 273 31 8.8 93811.64 13.49 0.604 0.629 89761- 61672 218 210 31 6.8 74954.07 11.96 0.497 0.325 61081- 47431 170 165 31 5.3 54309.72 9.57 0.496 0.422 47400- 1794 163 154 40 3.9 30302.03 6.47 0.603 0.540 ------------------------------------------------------------------------------------------- 3074982- 1794 3033 2906 319 9.1 347102.71 25.69 0.798 0.797 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 596 574 31 18.5 651739.77 48.16 0.788 0.849 0.015 1.05-0.83 539 527 32 16.5 403266.92 27.94 0.903 1.057 0.023 0.82-0.72 438 430 32 13.4 344011.21 23.22 0.787 0.864 0.029 0.72-0.65 373 358 32 11.2 252967.51 19.41 0.828 0.861 0.033 0.64-0.60 286 272 31 8.8 248020.27 17.98 0.821 0.908 0.035 0.59-0.56 254 239 35 6.8 154162.32 13.82 0.671 0.601 0.045 0.55-0.52 199 185 31 6.0 211027.39 16.92 0.670 0.630 0.040 0.51-0.49 155 145 31 4.7 131271.64 12.47 0.603 0.563 0.049 0.49-0.46 111 104 31 3.4 124184.07 12.60 0.463 0.363 0.050 0.45-0.40 82 72 33 2.2 114959.67 12.50 0.307 0.211 0.050 ------------------------------------------------------------------------------------------------------ inf-0.40 3033 2906 319 9.1 347102.71 25.69 0.798 0.797 0.025 inf-0.60 2206 2137 156 13.7 415857.00 29.84 0.823 0.904 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 574 31 31 100.0 18.5 651739.77 227.88 0.788 0.004 1.05-0.83 527 32 32 100.0 16.5 403266.92 136.54 0.903 0.008 0.82-0.72 430 32 32 100.0 13.4 344011.21 100.01 0.787 0.011 0.72-0.65 358 32 32 100.0 11.2 252967.51 81.77 0.828 0.014 0.64-0.60 272 31 31 100.0 8.8 248020.27 68.09 0.821 0.016 0.59-0.56 239 38 35 92.1 6.8 154162.32 46.02 0.671 0.023 0.55-0.52 185 36 31 86.1 6.0 211027.39 51.81 0.670 0.020 0.51-0.49 145 42 31 73.8 4.7 131271.64 31.26 0.603 0.027 0.49-0.46 104 57 31 54.4 3.4 124184.07 27.13 0.463 0.030 0.45-0.40 72 128 33 25.8 2.2 114959.67 20.76 0.307 0.032 -------------------------------------------------------------------------------------------- inf-0.40 2906 463 319 68.9 9.1 347102.71 111.15 0.798 0.013 inf-0.60 2137 156 156 100.0 13.7 415857.00 136.68 0.823 0.009 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: 0.015564 -0.079454 -0.025038 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029178 0.072511 ( 0.000007 0.000007 0.000006 ) -0.076552 -0.003634 -0.036245 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007185 0.000001 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007178 0.000005 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000005 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.015564 -0.079454 -0.025038 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029178 0.072511 ( 0.000007 0.000007 0.000006 ) -0.076552 -0.003634 -0.036245 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3682(5) 8.3723(7) 8.3601(6) 90.042(6) 89.998(5) 90.011(6) V = 585.71(7) unit cell: 8.36683(18) 8.36683(18) 8.36683(18) 90.0 90.0 90.0 V = 585.71(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) PROFFIT INFO: signal sum: min=235.0000 max=20917466.0000 PROFFIT INFO: signal sum lp corr: min=469.1951 max=2977048.4106 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=750.7121 max=4763277.5000 PROFFIT INFO: sig(Inet): min=120.4339 max=47821.4961 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 66 298 636 1248 1400 2492 4080 5590 6094 Percent 0.0 0.0 1.1 4.9 10.4 20.5 23.0 40.9 67.0 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4763278- 1126878 304 1857504.16 122.09 100.00 1120723- 632084 304 856456.38 102.98 100.00 631645- 267497 304 418560.97 94.92 100.00 267413- 170043 304 203629.39 70.39 100.00 170002- 120782 304 145593.02 51.27 100.00 120558- 94182 304 106661.93 36.29 100.00 94162- 67230 304 81545.53 29.59 100.00 67065- 5692 304 38005.19 19.24 100.00 5683- 2972 304 3973.94 5.40 97.04 2970- 751 311 2127.92 3.72 54.98 ------------------------------------------------------------------------------------ 4763278- 751 3047 370557.48 53.47 95.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 732009.62 93.49 100.00 1.41- 1.12 304 629558.85 63.27 99.34 1.12- 0.96 304 481168.78 70.27 97.70 0.96- 0.88 304 357423.02 60.14 94.74 0.88- 0.81 304 454296.32 68.89 99.34 0.81- 0.73 304 246715.90 41.11 95.72 0.73- 0.71 304 174260.73 33.81 87.17 0.71- 0.65 304 323112.42 48.53 95.07 0.65- 0.62 304 157003.25 27.68 87.17 0.62- 0.58 311 154989.68 28.13 94.86 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 370557.48 53.47 95.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:32:31 2018 Sorting 3047 observations 85 unique observations with > 7.00 F2/sig(F2) 3047 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 98 519 Total number of frames 519 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3047 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 2446 observations > 7.00 F2/sig(F2) 2446 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 26.3 (Out of 2446 removed 3 = 2443, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2443 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 93 unique data precomputed (should be 93) 93 unique data with 2443 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.3 (Out of 2443 removed 0 = 2443, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2443 observations RMS deviation of equivalent data = 0.26314 Rint = 0.18817 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18047, wR= 0.27579 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13648, wR= 0.17925, Acormin=0.601, Acormax=1.405, Acor_av=0.977 F test: Probability=1.000, F= 1.745 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11335, wR= 0.14644, Acormin=0.559, Acormax=1.478, Acor_av=0.913 F test: Probability=1.000, F= 1.448 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10725, wR= 0.14571, Acormin=0.581, Acormax=1.552, Acor_av=0.942 F test: Probability=0.995, F= 1.114 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08839, wR= 0.11934, Acormin=0.499, Acormax=1.574, Acor_av=0.878 F test: Probability=1.000, F= 1.470 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07681, wR= 0.10881, Acormin=0.473, Acormax=1.602, Acor_av=0.888 F test: Probability=1.000, F= 1.320 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10003, wR= 0.13854, Acormin=0.592, Acormax=1.613, Acor_av=0.950 F test: Probability=0.000, F= 0.589 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08189, wR= 0.11319, Acormin=0.481, Acormax=1.614, Acor_av=0.884 F test: Probability=0.000, F= 0.878 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07367, wR= 0.10384, Acormin=0.456, Acormax=1.628, Acor_av=0.894 F test: Probability=0.969, F= 1.081 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07215, wR= 0.10159, Acormin=0.320, Acormax=1.425, Acor_av=0.778 F test: Probability=0.812, F= 1.038 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09726, wR= 0.13468, Acormin=0.554, Acormax=1.597, Acor_av=0.922 F test: Probability=0.000, F= 0.572 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08142, wR= 0.11150, Acormin=0.459, Acormax=1.499, Acor_av=0.805 F test: Probability=0.000, F= 0.815 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07854, wR= 0.10610, Acormin=0.110, Acormax=0.398, Acor_av=0.215 F test: Probability=0.000, F= 0.873 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07185, wR= 0.09778, Acormin=0.120, Acormax=0.447, Acor_av=0.242 F test: Probability=0.818, F= 1.039 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06291, wR= 0.08919, Acormin=0.159, Acormax=0.499, Acor_av=0.260 F test: Probability=1.000, F= 1.346 Final absorption model (ne=6, no=3): Rint= 0.07367, Acormin=0.456, Acormax=1.628, Acor_av=0.894 Combined refinement in use Rint: 0.18828 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 114 pars with 6555 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26314 Using Levenberg-Marquardt: 0.00010 New wR= 0.06328 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18817 with corrections 0.05022 Rint for all data: 0.18828 with corrections 0.05044 0 observations identified as outliers and rejected Cycle 2 wR= 0.06328 Using Levenberg-Marquardt: 0.00001 New wR= 0.05849 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18817 with corrections 0.04601 Rint for all data: 0.18828 with corrections 0.04623 0 observations identified as outliers and rejected Cycle 3 wR= 0.05849 Using Levenberg-Marquardt: 0.00000 New wR= 0.05750 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18817 with corrections 0.04510 Rint for all data: 0.18828 with corrections 0.04533 0 observations identified as outliers and rejected Cycle 4 wR= 0.05750 Using Levenberg-Marquardt: 0.00000 New wR= 0.05701 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18817 with corrections 0.04463 Rint for all data: 0.18828 with corrections 0.04485 0 observations identified as outliers and rejected Cycle 5 wR= 0.05701 Using Levenberg-Marquardt: 0.00000 New wR= 0.05670 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18817 with corrections 0.04432 Rint for all data: 0.18828 with corrections 0.04454 0 observations identified as outliers and rejected Final wR= 0.05670 Final frame scales: Min= 0.7424 Max= 1.2871 Final absorption correction factors: Amin= 0.4866 Amax= 1.3483 PROFFIT INFO: Inet (after scale3 abspack): min=793.5172 max=4679938.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=108.3662 max=52484.1172 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 3047 reflections read from tmp file 601 reflections are rejected (601 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 4 1 3 0 5 5 85 Initial Chi^2= 0.39688 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.99488 Current error model SIG(F2)^2 = 166.32*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 331.80*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 331.80*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4679938- 1096821 304 1753826.83 81.36 100.00 1096429- 609879 304 815362.62 36.66 100.00 609085- 257685 304 404988.73 38.19 100.00 257385- 155208 304 192819.72 27.03 100.00 155160- 125628 304 140006.68 18.35 100.00 125614- 87705 304 102929.75 13.06 100.00 87584- 68969 304 78578.90 10.84 100.00 68945- 4950 304 40044.96 7.58 87.17 4934- 2751 304 3632.59 2.75 19.08 2749- 794 311 2146.84 2.27 10.61 ------------------------------------------------------------------------------------ 4679938- 794 3047 352626.73 23.76 81.52 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 734380.59 57.59 98.03 1.41- 1.12 304 612284.62 37.48 87.17 1.12- 0.96 304 440698.91 29.42 83.55 0.96- 0.88 304 335784.92 22.14 83.22 0.88- 0.81 304 428668.76 24.96 90.13 0.81- 0.73 304 228862.22 15.18 69.08 0.73- 0.71 304 162329.73 12.56 75.00 0.71- 0.65 304 299715.30 17.67 90.79 0.65- 0.62 304 146360.08 10.39 68.09 0.62- 0.58 311 142031.45 10.53 70.42 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 352626.73 23.76 81.52 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 734380.59 57.59 98.03 4.82- 1.12 608 673332.60 47.53 92.60 4.82- 0.96 912 595788.04 41.50 89.58 4.82- 0.88 1216 530787.26 36.66 87.99 4.82- 0.81 1520 510363.56 34.32 88.42 4.82- 0.73 1824 463446.67 31.13 85.20 4.82- 0.71 2128 420429.96 28.48 83.74 4.82- 0.65 2432 405340.63 27.13 84.62 4.82- 0.62 2736 376565.01 25.27 82.79 4.82- 0.58 3047 352626.73 23.76 81.52 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 352626.73 23.76 81.52 Scale applied to data: s=0.213678 (maximum obs:4679938.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.045; Rsigma 0.027: data 3047 -> merged 110 With outlier rejection... Rint 0.042; Rsigma 0.028: data 3030 -> merged 110 Rejected total: 17, method kkm 9, method Blessing 8 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585795, 4.830589 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 17.60 100.00 176 1.61 - 1.21 10 10 27.60 100.00 276 1.17 - 1.01 10 10 36.00 100.00 360 0.99 - 0.89 10 10 35.30 100.00 353 0.88 - 0.81 10 10 34.00 100.00 340 0.81 - 0.74 10 10 29.30 100.00 293 0.73 - 0.71 10 10 32.20 100.00 322 0.70 - 0.66 10 10 27.30 100.00 273 0.66 - 0.64 10 10 24.90 100.00 249 0.63 - 0.60 10 10 24.10 100.00 241 --------------------------------------------------------------- 5.92 - 0.60 100 100 28.83 100.00 2883 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:32:30 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917898 5.914164 5.913554 60.0465 90.0831 60.0348 2905 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.61 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1461 1523 1454 1463 2219 1954 1924 2905 N (int>3sigma) = 0 1199 1523 1192 1218 1957 1649 1614 2435 Mean intensity = 0.0 54.2 24.4 54.2 55.4 44.0 60.1 57.8 58.4 Mean int/sigma = 0.0 24.8 21.4 24.5 24.7 23.5 26.1 25.6 25.6 Lattice type: P chosen Volume: 146.42 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.914 90.06 119.94 119.95 Niggli form: a.a = 34.970 b.b = 34.977 c.c = 34.980 b.c = -0.034 a.c = -17.457 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.089 CUBIC F-lattice R(int) = 0.176 [ 2749] Vol = 585.7 Cell: 8.368 8.372 8.360 90.04 90.00 90.01 Volume: 585.70 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 2470] Vol = 439.3 Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.27 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.170 [ 788] Vol = 439.3 Trigonal Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.27 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.018 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.8 Cell: 5.919 5.918 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.049 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.8 Cell: 5.918 5.919 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.153 [ 2452] Vol = 292.8 Cell: 5.918 5.919 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.148 [ 2451] Vol = 292.8 Cell: 5.914 8.368 5.918 89.99 89.92 89.99 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.138 [ 2113] Vol = 292.8 Cell: 5.919 5.918 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.060 MONOCLINIC I-lattice R(int) = 0.139 [ 2114] Vol = 292.8 Cell: 5.914 5.918 8.368 90.01 90.01 89.92 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.007 MONOCLINIC I-lattice R(int) = 0.138 [ 2135] Vol = 292.8 Cell: 5.914 8.368 5.918 89.99 90.08 90.01 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.036 MONOCLINIC I-lattice R(int) = 0.131 [ 2112] Vol = 292.8 Cell: 5.918 5.914 8.368 89.99 90.01 90.08 Volume: 292.85 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.157 [ 2120] Vol = 292.8 Cell: 10.247 5.914 5.914 90.06 125.21 89.95 Volume: 292.85 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.117 [ 1528] Vol = 146.4 Cell: 5.914 5.914 5.914 90.06 119.94 119.95 Volume: 146.42 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1523 0 1956 1946 2905 N (int>3sigma) = 0 0 0 0 1523 0 1647 1647 2435 Mean intensity = 0.0 0.0 0.0 0.0 24.4 0.0 57.8 58.4 58.4 Mean int/sigma = 0.0 0.0 0.0 0.0 21.4 0.0 25.5 25.7 25.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.143 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 217 661 N I>3s 28 28 102 661 0.8 0.8 0.6 29.1 6.3 6.3 3.5 26.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.176 2552 Fd-3m 1 1 227 C N N N N 37 2284 0.176 2590 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368104 8.372165 8.360031 90.0421 89.9976 90.0109 ZERR 1.00 0.003434 0.001602 0.000272 0.0011 0.0115 0.0014 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3966901- 518832 673 662 27 24.5 1189999.02 54.69 0.038 0.044 506269- 119810 906 902 27 33.4 213524.06 26.84 0.049 0.069 107616- 35320 753 753 27 27.9 79101.93 10.81 0.067 0.089 10224- 1822 715 713 29 24.6 3502.42 2.73 0.167 0.229 ------------------------------------------------------------------------------------------- 3966901- 1822 3047 3030 110 27.5 344039.28 23.27 0.042 0.050 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 765 750 27 27.8 596747.47 43.01 0.036 0.038 0.016 1.01-0.78 911 911 27 33.7 338068.52 21.36 0.033 0.041 0.028 0.78-0.65 771 770 27 28.5 258214.36 16.12 0.055 0.068 0.041 0.65-0.59 600 599 29 20.7 147033.31 10.64 0.078 0.094 0.059 ------------------------------------------------------------------------------------------------------ inf-0.59 3047 3030 110 27.5 344039.28 23.27 0.042 0.050 0.028 inf-0.60 2897 2881 99 29.1 356056.38 23.98 0.041 0.048 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 750 27 27 100.0 27.8 596747.47 232.03 0.036 0.003 1.01-0.78 911 27 27 100.0 33.7 338068.52 125.25 0.033 0.005 0.78-0.65 770 27 27 100.0 28.5 258214.36 90.21 0.055 0.009 0.65-0.59 599 29 29 100.0 20.7 147033.31 54.43 0.078 0.018 -------------------------------------------------------------------------------------------- inf-0.59 3030 110 110 100.0 27.5 344039.28 128.77 0.042 0.006 inf-0.60 2881 99 99 100.0 29.1 356056.38 133.18 0.041 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:33:34 2018) ID: 2932; threads 40; handles 877; mem 520036.00 (1245892.00)kB; time: 1w 5d 0h 39m 4s MEMORY INFO: Memory PF:0.0, Ph:232.0, V:1216.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:507.8,peak PF: 697.1, WS: 298.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:232.0, V:1218.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:509.6,peak PF: 697.1, WS: 300.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:33:34 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.069967 0.030657 0.089101 ( 0.000011 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000011 0.000014 0.000012 ) 0.109112 -0.153091 0.115835 ( 0.000008 0.000010 0.000009 ) 5.91502 ( 0.00072 ) 5.91640 ( 0.00072 ) 5.92265 ( 0.00061 ) 60.05206 ( 0.01170 ) 89.98756 ( 0.00909 ) 60.01743 ( 0.01270 ) V = 146.73 Selected cell (from UM rr/UM ttt/UM f): 6 5.9150 5.9164 5.9227 60.0521 89.9876 60.0174 tI Cross checking gral lattice... Lattice type P selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 53.00 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:33:34 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.069967 0.030657 0.089101 ( 0.000011 0.000013 0.000012 ) -0.068858 -0.065594 -0.010716 ( 0.000011 0.000014 0.000012 ) 0.109112 -0.153091 0.115835 ( 0.000008 0.000010 0.000009 ) M - matrix: 0.021547 -0.014366 0.007205 ( 0.000003 0.000002 0.000002 ) -0.014366 0.028739 -0.014371 ( 0.000002 0.000004 0.000002 ) 0.007205 -0.014371 0.021574 ( 0.000002 0.000002 0.000003 ) unit cell: 5.9150(7) 5.9164(7) 5.9227(6) 60.052(12) 89.988(9) 60.017(13) V = 146.73(3) Lattice type P used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) UB fit with 633 obs out of 684 (total:685,skipped:1) (92.54%) UB - matrix: -0.070248 0.030900 0.088638 ( 0.000056 0.000066 0.000037 ) -0.067981 -0.066149 -0.010677 ( 0.000060 0.000071 0.000040 ) 0.109085 -0.152964 0.116274 ( 0.000082 0.000097 0.000054 ) M - matrix: 0.021456 -0.014360 0.007183 ( 0.000021 0.000018 0.000013 ) -0.014360 0.028728 -0.014341 ( 0.000018 0.000032 0.000016 ) 0.007183 -0.014341 0.021490 ( 0.000013 0.000016 0.000014 ) unit cell: 5.936(4) 5.920(4) 5.925(3) 60.06(6) 90.06(4) 59.95(7) V = 147.18(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.070195 0.030773 0.088467 ( 0.000058 0.000068 0.000038 ) -0.068017 -0.065940 -0.010654 ( 0.000056 0.000066 0.000037 ) 0.108931 -0.152658 0.115911 ( 0.000074 0.000088 0.000049 ) M - matrix: 0.021420 -0.014304 0.007141 ( 0.000020 0.000017 0.000012 ) -0.014304 0.028600 -0.014270 ( 0.000017 0.000028 0.000014 ) 0.007141 -0.014270 0.021375 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.939(3) 5.933(4) 5.941(3) 60.03(6) 90.02(4) 59.96(6) V = 147.97(12) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 810 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070202 0.030775 0.088468 ( 0.000059 0.000069 0.000039 ) -0.068028 -0.065928 -0.010657 ( 0.000056 0.000066 0.000037 ) 0.108946 -0.152671 0.115913 ( 0.000075 0.000088 0.000049 ) M - matrix: 0.021425 -0.014308 0.007143 ( 0.000020 0.000017 0.000012 ) -0.014308 0.028602 -0.014271 ( 0.000017 0.000028 0.000014 ) 0.007143 -0.014271 0.021376 ( 0.000012 0.000014 0.000013 ) UB fit with 638 obs out of 684 (total:685,skipped:1) (93.27%) unit cell: 5.938(3) 5.933(4) 5.941(3) 60.03(6) 90.01(4) 59.96(6) V = 147.96(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 637 obs out of 684 (total:685,skipped:1) (93.13%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 44 | 0.992 ( 0.203) | 1.322 ( 0.746) | 1.711 ( 2.368) | 1.33- 1.09 | 44 | 1.058 ( 0.121) | 1.080 ( 0.153) | 1.111 ( 0.494) | 1.09- 0.96 | 44 | 1.061 ( 0.106) | 1.080 ( 0.132) | 1.088 ( 0.418) | 0.96- 0.84 | 44 | 1.076 ( 0.113) | 1.068 ( 0.141) | 1.123 ( 0.382) | 0.84- 0.81 | 44 | 1.108 ( 0.099) | 1.025 ( 0.123) | 1.394 ( 0.507) | 0.81- 0.73 | 44 | 1.095 ( 0.087) | 0.996 ( 0.125) | 1.301 ( 0.497) | 0.73- 0.70 | 44 | 1.087 ( 0.079) | 0.930 ( 0.110) | 1.408 ( 0.497) | 0.69- 0.66 | 44 | 1.082 ( 0.073) | 0.885 ( 0.089) | 1.376 ( 0.479) | 0.66- 0.63 | 44 | 1.064 ( 0.067) | 0.862 ( 0.062) | 1.444 ( 0.591) | 0.63- 0.59 | 47 | 1.015 ( 0.089) | 0.817 ( 0.076) | 1.286 ( 0.540) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 443 | 1.063 ( 0.115) | 1.005 ( 0.294) | 1.324 ( 0.899) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) UB - matrix: -0.070033 0.030485 0.088659 ( 0.000027 0.000026 0.000015 ) -0.068377 -0.065762 -0.010702 ( 0.000027 0.000027 0.000015 ) 0.109069 -0.152751 0.115661 ( 0.000027 0.000027 0.000016 ) M - matrix: 0.021476 -0.014299 0.007138 ( 0.000008 0.000006 0.000005 ) -0.014299 0.028587 -0.014261 ( 0.000006 0.000009 0.000005 ) 0.007138 -0.014261 0.021352 ( 0.000005 0.000005 0.000005 ) unit cell: 5.9265(15) 5.9308(15) 5.9443(11) 60.01(2) 90.019(18) 60.02(3) V = 147.79(5) OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 OTKP changes: 443 1 1 1 UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=53.000) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070132 0.030659 0.088729 ( 0.000024 0.000024 0.000014 ) -0.068216 -0.065963 -0.010732 ( 0.000025 0.000025 0.000014 ) 0.109143 -0.152997 0.116004 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021484 -0.014349 0.007170 ( 0.000007 0.000005 0.000004 ) -0.014349 0.028699 -0.014320 ( 0.000005 0.000008 0.000004 ) 0.007170 -0.014320 0.021445 ( 0.000004 0.000004 0.000004 ) UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) unit cell: 5.9294(14) 5.9217(14) 5.9315(10) 60.04(2) 90.042(16) 59.98(2) V = 147.26(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 443 obs out of 443 (total:443,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 450 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 1.32 | 44 | 0.974 ( 0.155) | 1.302 ( 0.737) | 1.284 ( 0.802) | 1.32- 1.09 | 44 | 1.062 ( 0.111) | 1.083 ( 0.139) | 1.171 ( 0.506) | 1.09- 0.96 | 44 | 1.067 ( 0.101) | 1.087 ( 0.141) | 1.124 ( 0.474) | 0.96- 0.84 | 44 | 1.072 ( 0.111) | 1.054 ( 0.135) | 1.145 ( 0.402) | 0.84- 0.81 | 44 | 1.112 ( 0.098) | 1.030 ( 0.131) | 1.355 ( 0.481) | 0.81- 0.73 | 44 | 1.086 ( 0.088) | 0.994 ( 0.129) | 1.305 ( 0.486) | 0.73- 0.70 | 44 | 1.094 ( 0.076) | 0.949 ( 0.112) | 1.402 ( 0.488) | 0.70- 0.67 | 44 | 1.077 ( 0.071) | 0.883 ( 0.070) | 1.422 ( 0.488) | 0.67- 0.63 | 44 | 1.074 ( 0.063) | 0.865 ( 0.062) | 1.481 ( 0.585) | 0.63- 0.59 | 46 | 1.008 ( 0.079) | 0.805 ( 0.036) | 1.270 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.79- 0.59 | 442 | 1.062 ( 0.106) | 1.004 ( 0.289) | 1.296 ( 0.543) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) UB fit with 509 obs out of 535 (total:535,skipped:0) (95.14%) UB - matrix: -0.070256 0.031221 0.088397 ( 0.000056 0.000045 0.000051 ) -0.068770 -0.065605 -0.010632 ( 0.000064 0.000051 0.000059 ) 0.108942 -0.152884 0.116118 ( 0.000076 0.000061 0.000070 ) M - matrix: 0.021534 -0.014337 0.007171 ( 0.000020 0.000015 0.000014 ) -0.014337 0.028652 -0.014295 ( 0.000015 0.000020 0.000014 ) 0.007171 -0.014295 0.021410 ( 0.000014 0.000014 0.000019 ) unit cell: 5.919(3) 5.923(3) 5.936(3) 60.04(5) 90.07(4) 60.04(6) V = 147.23(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) UB - matrix: -0.070134 0.031107 0.088435 ( 0.000053 0.000043 0.000049 ) -0.068518 -0.065603 -0.010538 ( 0.000063 0.000051 0.000058 ) 0.108827 -0.152550 0.116092 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021457 -0.014288 0.007154 ( 0.000020 0.000015 0.000014 ) -0.014288 0.028543 -0.014267 ( 0.000015 0.000020 0.000014 ) 0.007154 -0.014267 0.021409 ( 0.000014 0.000014 0.000019 ) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.03(5) 90.05(4) 60.02(6) V = 147.80(12) OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 OTKP changes: 99 1 1 1 UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 737 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070130 0.031111 0.088442 ( 0.000053 0.000043 0.000049 ) -0.068509 -0.065610 -0.010528 ( 0.000063 0.000051 0.000058 ) 0.108821 -0.152526 0.116086 ( 0.000077 0.000062 0.000071 ) M - matrix: 0.021454 -0.014285 0.007151 ( 0.000020 0.000015 0.000014 ) -0.014285 0.028537 -0.014264 ( 0.000015 0.000020 0.000014 ) 0.007151 -0.014264 0.021409 ( 0.000014 0.000014 0.000019 ) UB fit with 511 obs out of 535 (total:535,skipped:0) (95.51%) unit cell: 5.931(3) 5.936(3) 5.936(3) 60.04(5) 90.04(4) 60.01(6) V = 147.82(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 510 obs out of 535 (total:535,skipped:0) (95.33%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 411 peaks identified as outliers and rejected 407 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 407 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 407 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 1.33 | 41 | 0.980 ( 0.145) | 1.253 ( 0.664) | 1.206 ( 0.998) | 1.33- 1.09 | 41 | 1.018 ( 0.087) | 1.088 ( 0.108) | 1.025 ( 0.397) | 1.09- 0.96 | 41 | 1.030 ( 0.085) | 1.111 ( 0.124) | 1.064 ( 0.463) | 0.94- 0.84 | 41 | 1.006 ( 0.088) | 1.059 ( 0.140) | 1.087 ( 0.414) | 0.84- 0.81 | 41 | 1.012 ( 0.082) | 1.046 ( 0.140) | 1.064 ( 0.290) | 0.81- 0.73 | 41 | 0.986 ( 0.062) | 1.040 ( 0.152) | 1.067 ( 0.365) | 0.73- 0.70 | 41 | 0.968 ( 0.058) | 0.951 ( 0.166) | 1.128 ( 0.459) | 0.69- 0.66 | 41 | 0.962 ( 0.041) | 0.911 ( 0.093) | 1.220 ( 0.444) | 0.66- 0.63 | 41 | 0.923 ( 0.028) | 0.854 ( 0.042) | 1.231 ( 0.483) | 0.63- 0.59 | 38 | 0.893 ( 0.032) | 0.828 ( 0.059) | 1.248 ( 0.453) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.75- 0.59 | 407 | 0.978 ( 0.088) | 1.015 ( 0.269) | 1.133 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) UB - matrix: -0.070154 0.031011 0.088690 ( 0.000023 0.000020 0.000025 ) -0.068248 -0.065884 -0.010255 ( 0.000031 0.000027 0.000033 ) 0.108861 -0.152411 0.116306 ( 0.000023 0.000020 0.000024 ) M - matrix: 0.021430 -0.014271 0.007139 ( 0.000007 0.000005 0.000005 ) -0.014271 0.028532 -0.014300 ( 0.000005 0.000007 0.000005 ) 0.007139 -0.014300 0.021498 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9331(16) 5.9393(16) 5.9251(13) 59.97(3) 89.95(2) 59.99(3) V = 147.62(6) OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 OTKP changes: 407 1 1 1 UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.000) HKL list info: 733 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070288 0.031126 0.088599 ( 0.000023 0.000019 0.000024 ) -0.068470 -0.065861 -0.010354 ( 0.000029 0.000025 0.000031 ) 0.108974 -0.152724 0.116322 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021504 -0.014321 0.007158 ( 0.000007 0.000005 0.000005 ) -0.014321 0.028631 -0.014325 ( 0.000005 0.000006 0.000005 ) 0.007158 -0.014325 0.021488 ( 0.000005 0.000005 0.000006 ) UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) unit cell: 5.9231(15) 5.9292(15) 5.9273(12) 59.97(2) 89.968(18) 60.00(3) V = 147.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 407 obs out of 407 (total:407,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 407 peaks identified as outliers and rejected 404 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 404 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 404 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 40 | 0.984 ( 0.141) | 1.253 ( 0.686) | 1.194 ( 0.956) | 1.32- 1.09 | 40 | 1.024 ( 0.082) | 1.092 ( 0.108) | 1.061 ( 0.429) | 1.09- 0.97 | 40 | 1.018 ( 0.090) | 1.149 ( 0.370) | 1.055 ( 0.434) | 0.96- 0.88 | 40 | 1.001 ( 0.090) | 1.050 ( 0.141) | 1.050 ( 0.402) | 0.88- 0.81 | 40 | 1.022 ( 0.078) | 1.058 ( 0.141) | 1.057 ( 0.240) | 0.81- 0.73 | 40 | 0.979 ( 0.067) | 1.047 ( 0.151) | 1.080 ( 0.403) | 0.73- 0.71 | 40 | 0.979 ( 0.056) | 0.949 ( 0.118) | 1.201 ( 0.566) | 0.71- 0.67 | 40 | 0.963 ( 0.039) | 0.904 ( 0.077) | 1.214 ( 0.475) | 0.67- 0.63 | 40 | 0.923 ( 0.032) | 0.859 ( 0.065) | 1.162 ( 0.437) | 0.63- 0.59 | 44 | 0.898 ( 0.036) | 0.834 ( 0.061) | 1.272 ( 0.459) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 404 | 0.978 ( 0.087) | 1.018 ( 0.294) | 1.136 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.023 ( 0.233) | 1.207 ( 0.649) | 1.113 ( 0.620) | 1.41- 1.17 | 48 | 1.019 ( 0.089) | 1.074 ( 0.177) | 0.911 ( 0.378) | 1.17- 1.01 | 48 | 0.997 ( 0.092) | 1.081 ( 0.362) | 1.011 ( 0.447) | 1.01- 0.92 | 48 | 1.024 ( 0.072) | 1.024 ( 0.107) | 1.102 ( 0.434) | 0.92- 0.82 | 48 | 0.999 ( 0.081) | 0.976 ( 0.107) | 1.105 ( 0.378) | 0.82- 0.75 | 48 | 0.993 ( 0.080) | 0.963 ( 0.115) | 1.087 ( 0.437) | 0.75- 0.71 | 48 | 0.983 ( 0.046) | 0.920 ( 0.070) | 1.220 ( 0.515) | 0.71- 0.66 | 48 | 0.951 ( 0.047) | 0.861 ( 0.054) | 1.234 ( 0.482) | 0.66- 0.62 | 48 | 0.934 ( 0.048) | 0.844 ( 0.038) | 1.181 ( 0.432) | 0.62- 0.59 | 48 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.354 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 480 | 0.983 ( 0.106) | 0.976 ( 0.277) | 1.132 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) UB fit with 629 obs out of 669 (total:669,skipped:0) (94.02%) UB - matrix: -0.069833 0.031223 0.088934 ( 0.000048 0.000072 0.000055 ) -0.068712 -0.065609 -0.010008 ( 0.000044 0.000067 0.000051 ) 0.109008 -0.152983 0.116410 ( 0.000062 0.000094 0.000071 ) M - matrix: 0.021481 -0.014349 0.007167 ( 0.000016 0.000016 0.000013 ) -0.014349 0.028683 -0.014375 ( 0.000016 0.000030 0.000017 ) 0.007167 -0.014375 0.021561 ( 0.000013 0.000017 0.000019 ) unit cell: 5.931(3) 5.931(3) 5.920(3) 59.93(6) 89.90(4) 59.93(6) V = 147.04(13) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) UB - matrix: -0.069903 0.031166 0.088855 ( 0.000045 0.000068 0.000052 ) -0.068741 -0.065502 -0.009992 ( 0.000042 0.000064 0.000048 ) 0.108759 -0.152855 0.116282 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021440 -0.014300 0.007122 ( 0.000017 0.000016 0.000013 ) -0.014300 0.028626 -0.014351 ( 0.000016 0.000032 0.000018 ) 0.007122 -0.014351 0.021517 ( 0.000013 0.000018 0.000020 ) unit cell: 5.932(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069931 0.031164 0.088851 ( 0.000045 0.000068 0.000052 ) -0.068752 -0.065495 -0.010013 ( 0.000042 0.000064 0.000048 ) 0.108746 -0.152847 0.116261 ( 0.000066 0.000100 0.000076 ) M - matrix: 0.021443 -0.014298 0.007118 ( 0.000017 0.000016 0.000013 ) -0.014298 0.028623 -0.014345 ( 0.000016 0.000032 0.000018 ) 0.007118 -0.014345 0.021511 ( 0.000013 0.000018 0.000020 ) UB fit with 625 obs out of 669 (total:669,skipped:0) (93.42%) unit cell: 5.931(3) 5.936(3) 5.927(3) 59.86(6) 89.81(4) 59.95(6) V = 147.39(12) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 623 obs out of 669 (total:669,skipped:0) (93.12%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 10 of 484 peaks identified as outliers and rejected 474 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 474 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 474 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.032 ( 0.144) | 1.122 ( 0.424) | 1.109 ( 0.575) | 1.41- 1.12 | 47 | 1.052 ( 0.100) | 1.275 ( 0.643) | 1.092 ( 0.634) | 1.12- 0.98 | 47 | 1.019 ( 0.102) | 1.057 ( 0.160) | 0.964 ( 0.364) | 0.98- 0.89 | 47 | 1.029 ( 0.093) | 1.035 ( 0.135) | 1.097 ( 0.433) | 0.89- 0.82 | 47 | 1.036 ( 0.085) | 1.007 ( 0.124) | 1.151 ( 0.478) | 0.82- 0.75 | 47 | 1.038 ( 0.080) | 0.984 ( 0.119) | 1.196 ( 0.514) | 0.75- 0.71 | 47 | 1.027 ( 0.045) | 0.938 ( 0.113) | 1.296 ( 0.513) | 0.71- 0.67 | 47 | 1.001 ( 0.040) | 0.889 ( 0.071) | 1.260 ( 0.499) | 0.67- 0.63 | 47 | 0.974 ( 0.043) | 0.842 ( 0.039) | 1.301 ( 0.513) | 0.63- 0.59 | 51 | 0.945 ( 0.054) | 0.815 ( 0.041) | 1.344 ( 0.525) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 474 | 1.015 ( 0.091) | 0.995 ( 0.292) | 1.182 ( 0.522) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) UB - matrix: -0.070174 0.031436 0.088653 ( 0.000017 0.000026 0.000022 ) -0.068860 -0.065672 -0.010206 ( 0.000019 0.000030 0.000026 ) 0.108880 -0.152867 0.116127 ( 0.000017 0.000026 0.000022 ) M - matrix: 0.021521 -0.014328 0.007126 ( 0.000005 0.000005 0.000004 ) -0.014328 0.028669 -0.014295 ( 0.000005 0.000009 0.000005 ) 0.007126 -0.014295 0.021449 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9190(15) 5.9207(15) 5.9270(11) 60.01(2) 89.926(18) 59.98(3) V = 146.96(5) OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 OTKP changes: 474 1 1 1 UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=53.000) HKL list info: 794 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069916 0.031387 0.088700 ( 0.000016 0.000025 0.000021 ) -0.068769 -0.065667 -0.010009 ( 0.000017 0.000026 0.000022 ) 0.108887 -0.152875 0.116249 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021474 -0.014325 0.007145 ( 0.000005 0.000005 0.000004 ) -0.014325 0.028668 -0.014330 ( 0.000005 0.000009 0.000005 ) 0.007145 -0.014330 0.021482 ( 0.000004 0.000005 0.000006 ) UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) unit cell: 5.9281(13) 5.9264(13) 5.9276(11) 59.97(2) 89.937(16) 59.98(2) V = 147.21(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 474 obs out of 474 (total:474,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.030 ( 0.150) | 1.116 ( 0.422) | 1.104 ( 0.741) | 1.41- 1.12 | 47 | 1.047 ( 0.097) | 1.280 ( 0.655) | 1.108 ( 0.646) | 1.12- 0.97 | 47 | 1.014 ( 0.108) | 1.028 ( 0.130) | 0.949 ( 0.328) | 0.97- 0.89 | 47 | 1.028 ( 0.089) | 1.029 ( 0.137) | 1.105 ( 0.406) | 0.88- 0.82 | 47 | 1.047 ( 0.079) | 1.022 ( 0.118) | 1.207 ( 0.509) | 0.82- 0.75 | 47 | 1.037 ( 0.080) | 0.987 ( 0.126) | 1.069 ( 0.407) | 0.75- 0.71 | 47 | 1.022 ( 0.044) | 0.934 ( 0.110) | 1.339 ( 0.543) | 0.71- 0.67 | 47 | 0.997 ( 0.043) | 0.885 ( 0.072) | 1.211 ( 0.465) | 0.67- 0.63 | 47 | 0.974 ( 0.047) | 0.841 ( 0.041) | 1.288 ( 0.498) | 0.63- 0.59 | 49 | 0.949 ( 0.045) | 0.812 ( 0.041) | 1.347 ( 0.519) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 472 | 1.014 ( 0.090) | 0.993 ( 0.294) | 1.173 ( 0.533) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 523 obs out of 550 (total:550,skipped:0) (95.09%) UB - matrix: -0.069499 0.031165 0.088917 ( 0.000043 0.000070 0.000062 ) -0.069000 -0.065444 -0.010175 ( 0.000031 0.000051 0.000045 ) 0.108929 -0.152990 0.116088 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021457 -0.014315 0.007168 ( 0.000013 0.000013 0.000012 ) -0.014315 0.028660 -0.014323 ( 0.000013 0.000026 0.000016 ) 0.007168 -0.014323 0.021486 ( 0.000012 0.000016 0.000020 ) unit cell: 5.930(3) 5.923(3) 5.926(3) 60.03(5) 90.05(4) 60.02(5) V = 147.23(11) UB fit with 523 obs out of 550 (total:550,skipped:0) (95.09%) UB - matrix: -0.069499 0.031165 0.088917 ( 0.000043 0.000070 0.000062 ) -0.069000 -0.065444 -0.010175 ( 0.000031 0.000051 0.000045 ) 0.108929 -0.152990 0.116088 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021457 -0.014315 0.007168 ( 0.000013 0.000013 0.000012 ) -0.014315 0.028660 -0.014323 ( 0.000013 0.000026 0.000016 ) 0.007168 -0.014323 0.021486 ( 0.000012 0.000016 0.000020 ) unit cell: 5.930(3) 5.923(3) 5.926(3) 60.03(5) 90.05(4) 60.02(5) V = 147.23(11) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069606 0.031383 0.088757 ( 0.000043 0.000071 0.000063 ) -0.068812 -0.065492 -0.010050 ( 0.000032 0.000053 0.000047 ) 0.109003 -0.152943 0.116137 ( 0.000049 0.000080 0.000071 ) M - matrix: 0.021462 -0.014349 0.007173 ( 0.000013 0.000013 0.000012 ) -0.014349 0.028666 -0.014319 ( 0.000013 0.000026 0.000016 ) 0.007173 -0.014319 0.021466 ( 0.000012 0.000016 0.000020 ) UB fit with 527 obs out of 550 (total:550,skipped:0) (95.82%) unit cell: 5.936(3) 5.928(3) 5.929(3) 60.04(5) 90.02(4) 59.93(5) V = 147.43(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 526 obs out of 550 (total:550,skipped:0) (95.64%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 451 peaks identified as outliers and rejected 448 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 448 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 448 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.48 | 45 | 0.999 ( 0.191) | 1.283 ( 0.753) | 1.137 ( 0.704) | 1.47- 1.17 | 45 | 1.014 ( 0.087) | 1.064 ( 0.193) | 0.971 ( 0.388) | 1.17- 0.98 | 45 | 1.007 ( 0.082) | 1.020 ( 0.115) | 0.971 ( 0.404) | 0.98- 0.92 | 45 | 0.998 ( 0.077) | 0.997 ( 0.120) | 1.059 ( 0.407) | 0.89- 0.82 | 45 | 1.013 ( 0.065) | 0.976 ( 0.102) | 1.258 ( 0.536) | 0.82- 0.75 | 45 | 0.990 ( 0.079) | 0.973 ( 0.124) | 1.109 ( 0.415) | 0.75- 0.71 | 45 | 0.972 ( 0.047) | 0.921 ( 0.064) | 1.238 ( 0.437) | 0.71- 0.67 | 45 | 0.948 ( 0.043) | 0.870 ( 0.063) | 1.252 ( 0.513) | 0.67- 0.62 | 45 | 0.912 ( 0.034) | 0.839 ( 0.045) | 1.384 ( 0.529) | 0.62- 0.59 | 43 | 0.885 ( 0.033) | 0.814 ( 0.038) | 1.452 ( 0.610) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 448 | 0.974 ( 0.096) | 0.976 ( 0.289) | 1.182 ( 0.527) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) UB - matrix: -0.069868 0.031444 0.088851 ( 0.000020 0.000034 0.000027 ) -0.068937 -0.065439 -0.010099 ( 0.000017 0.000028 0.000023 ) 0.109191 -0.152972 0.116370 ( 0.000018 0.000030 0.000024 ) M - matrix: 0.021557 -0.014389 0.007195 ( 0.000005 0.000005 0.000005 ) -0.014389 0.028672 -0.014347 ( 0.000005 0.000010 0.000006 ) 0.007195 -0.014347 0.021538 ( 0.000005 0.000006 0.000007 ) unit cell: 5.9241(14) 5.9300(14) 5.9191(13) 60.02(2) 89.980(19) 59.90(2) V = 146.89(5) OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 OTKP changes: 448 1 1 1 UB - matrix: -0.069613 0.031297 0.088856 ( 0.000019 0.000032 0.000026 ) -0.068939 -0.065449 -0.010080 ( 0.000017 0.000028 0.000023 ) 0.109040 -0.153008 0.116186 ( 0.000014 0.000024 0.000019 ) M - matrix: 0.021488 -0.014351 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014351 0.028674 -0.014337 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014337 0.021496 ( 0.000004 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9302(14) 5.9268(14) 5.9256(13) 60.02(2) 90.013(19) 59.96(2) V = 147.19(5) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=53.000) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069613 0.031297 0.088856 ( 0.000019 0.000032 0.000026 ) -0.068939 -0.065449 -0.010080 ( 0.000017 0.000028 0.000023 ) 0.109040 -0.153008 0.116186 ( 0.000014 0.000024 0.000019 ) M - matrix: 0.021488 -0.014351 0.007178 ( 0.000005 0.000005 0.000004 ) -0.014351 0.028674 -0.014337 ( 0.000005 0.000008 0.000005 ) 0.007178 -0.014337 0.021496 ( 0.000004 0.000005 0.000006 ) UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) unit cell: 5.9302(14) 5.9268(14) 5.9256(13) 60.02(2) 90.013(19) 59.96(2) V = 147.19(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 448 obs out of 448 (total:448,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 455 peaks identified as outliers and rejected 452 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 452 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 452 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 45 | 0.996 ( 0.196) | 1.198 ( 0.653) | 1.142 ( 0.733) | 1.48- 1.17 | 45 | 1.016 ( 0.088) | 1.087 ( 0.336) | 0.977 ( 0.385) | 1.17- 0.99 | 45 | 1.007 ( 0.081) | 1.044 ( 0.122) | 0.963 ( 0.386) | 0.99- 0.92 | 45 | 0.998 ( 0.081) | 1.001 ( 0.112) | 1.011 ( 0.408) | 0.92- 0.82 | 45 | 1.009 ( 0.070) | 0.966 ( 0.103) | 1.286 ( 0.515) | 0.82- 0.76 | 45 | 0.996 ( 0.078) | 0.976 ( 0.125) | 1.121 ( 0.441) | 0.76- 0.71 | 45 | 0.971 ( 0.051) | 0.930 ( 0.077) | 1.217 ( 0.451) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.879 ( 0.064) | 1.279 ( 0.537) | 0.67- 0.63 | 45 | 0.915 ( 0.035) | 0.844 ( 0.043) | 1.404 ( 0.536) | 0.63- 0.59 | 47 | 0.887 ( 0.034) | 0.813 ( 0.037) | 1.429 ( 0.608) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 452 | 0.974 ( 0.097) | 0.973 ( 0.269) | 1.184 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.2 | 225 | 1.115 ( 0.122) | 1.218 ( 0.427) | 1.170 ( 0.589) | 13.2-19.0 | 225 | 1.077 ( 0.053) | 1.130 ( 0.276) | 1.185 ( 0.517) | 19.0-23.1 | 225 | 1.064 ( 0.071) | 1.146 ( 0.399) | 1.184 ( 0.536) | 23.1-27.1 | 225 | 1.032 ( 0.076) | 1.065 ( 0.256) | 1.172 ( 0.558) | 27.2-30.8 | 225 | 1.009 ( 0.071) | 1.005 ( 0.235) | 1.183 ( 0.489) | 30.8-33.8 | 225 | 0.978 ( 0.079) | 0.940 ( 0.231) | 1.207 ( 0.515) | 33.8-36.9 | 225 | 0.959 ( 0.075) | 0.901 ( 0.106) | 1.175 ( 0.481) | 36.9-39.6 | 225 | 0.944 ( 0.085) | 0.870 ( 0.131) | 1.215 ( 0.553) | 39.7-42.7 | 225 | 0.920 ( 0.075) | 0.834 ( 0.078) | 1.206 ( 0.549) | 42.7-49.9 | 225 | 0.927 ( 0.085) | 0.810 ( 0.065) | 1.141 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2250 | 1.002 ( 0.103) | 0.992 ( 0.285) | 1.184 ( 0.527) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0024 b=1.00 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5030 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 706959 Maximum peak integral for reflections I/sig<= 10000 - raw: 10984832 lp-corr: 3692449 PROFFITPEAK - Finished at Tue Mar 27 15:33:57 2018 PROFFITMAIN - Started at Tue Mar 27 15:33:57 2018 OTKP changes: 2250 2 4 5 OTKP changes: 2250 2 4 5 UB - matrix: -0.070073 0.031150 0.088955 ( 0.000011 0.000013 0.000012 ) -0.068746 -0.065897 -0.010384 ( 0.000010 0.000012 0.000011 ) 0.109189 -0.153089 0.116378 ( 0.000009 0.000010 0.000009 ) M - matrix: 0.021558 -0.014368 0.007188 ( 0.000003 0.000002 0.000002 ) -0.014368 0.028749 -0.014361 ( 0.000002 0.000004 0.000002 ) 0.007188 -0.014361 0.021565 ( 0.000002 0.000002 0.000003 ) UB fit with 2250 obs out of 2250 (total:2250,skipped:0) (100.00%) unit cell: 5.9155(7) 5.9120(7) 5.9127(6) 60.051(11) 90.041(9) 60.018(12) V = 146.32(2) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) UB - matrix: -0.070073 0.030679 0.088931 ( 0.000028 0.000028 0.000016 ) -0.068224 -0.066129 -0.010545 ( 0.000025 0.000024 0.000014 ) 0.109089 -0.153071 0.116009 ( 0.000024 0.000024 0.000014 ) M - matrix: 0.021465 -0.014337 0.007143 ( 0.000007 0.000006 0.000004 ) -0.014337 0.028745 -0.014332 ( 0.000006 0.000008 0.000004 ) 0.007143 -0.014332 0.021478 ( 0.000004 0.000004 0.000004 ) unit cell: 5.9284(14) 5.9142(14) 5.9248(11) 60.02(2) 89.980(17) 59.99(2) V = 146.95(5) OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 OTKP changes: 442 1 1 1 UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109366 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109366 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* UB - matrix: -0.070372 0.030966 0.088817 ( 0.000026 0.000026 0.000015 ) -0.068400 -0.066171 -0.010642 ( 0.000024 0.000023 0.000013 ) 0.109366 -0.153305 0.116387 ( 0.000023 0.000023 0.000013 ) M - matrix: 0.021592 -0.014419 0.007206 ( 0.000007 0.000005 0.000004 ) -0.014419 0.028840 -0.014388 ( 0.000005 0.000008 0.000004 ) 0.007206 -0.014388 0.021548 ( 0.000004 0.000004 0.000004 ) UB fit with 442 obs out of 442 (total:442,skipped:0) (100.00%) unit cell: 5.9145(13) 5.9066(13) 5.9171(10) 60.04(2) 90.051(16) 59.99(2) V = 146.17(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) UB - matrix: -0.070405 0.031323 0.088620 ( 0.000025 0.000022 0.000027 ) -0.068591 -0.065973 -0.010269 ( 0.000031 0.000027 0.000033 ) 0.109002 -0.152698 0.116261 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021543 -0.014324 0.007138 ( 0.000007 0.000005 0.000005 ) -0.014324 0.028650 -0.014299 ( 0.000005 0.000006 0.000005 ) 0.007138 -0.014299 0.021476 ( 0.000005 0.000005 0.000007 ) unit cell: 5.9147(16) 5.9212(16) 5.9235(13) 60.02(3) 89.95(2) 60.01(3) V = 146.82(6) OTKP changes: 404 1 1 1 OTKP changes: 404 1 1 1 OTKP changes: 404 1 1 1 UB - matrix: -0.070379 0.031253 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068831 -0.065836 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153163 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014389 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014389 0.028770 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) HKL list info: 720 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070379 0.031253 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068831 -0.065836 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153163 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014389 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014389 0.028770 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* UB - matrix: -0.070379 0.031253 0.088846 ( 0.000023 0.000020 0.000025 ) -0.068831 -0.065836 -0.010382 ( 0.000030 0.000026 0.000032 ) 0.109173 -0.153163 0.116612 ( 0.000020 0.000017 0.000021 ) M - matrix: 0.021610 -0.014389 0.007193 ( 0.000007 0.000005 0.000005 ) -0.014389 0.028770 -0.014400 ( 0.000005 0.000006 0.000005 ) 0.007193 -0.014400 0.021600 ( 0.000005 0.000005 0.000007 ) UB fit with 404 obs out of 404 (total:404,skipped:0) (100.00%) unit cell: 5.9082(16) 5.9151(16) 5.9125(12) 59.96(2) 89.961(19) 60.01(3) V = 146.08(5) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb Run 3 has been already processed *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) UB - matrix: -0.070118 0.031473 0.088650 ( 0.000016 0.000025 0.000021 ) -0.068840 -0.065724 -0.010157 ( 0.000020 0.000031 0.000026 ) 0.108946 -0.152898 0.116187 ( 0.000016 0.000025 0.000021 ) M - matrix: 0.021525 -0.014340 0.007141 ( 0.000005 0.000005 0.000004 ) -0.014340 0.028688 -0.014307 ( 0.000005 0.000009 0.000005 ) 0.007141 -0.014307 0.021461 ( 0.000004 0.000005 0.000006 ) unit cell: 5.9198(15) 5.9195(15) 5.9260(11) 60.02(2) 89.959(17) 59.98(3) V = 146.91(5) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 UB - matrix: -0.070175 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066049 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9142(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.070175 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066049 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9142(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* UB - matrix: -0.070175 0.031470 0.088879 ( 0.000016 0.000025 0.000021 ) -0.068740 -0.066049 -0.009944 ( 0.000018 0.000028 0.000024 ) 0.109193 -0.153149 0.116602 ( 0.000016 0.000024 0.000020 ) M - matrix: 0.021573 -0.014391 0.007179 ( 0.000005 0.000005 0.000004 ) -0.014391 0.028807 -0.014404 ( 0.000005 0.000008 0.000005 ) 0.007179 -0.014404 0.021594 ( 0.000004 0.000005 0.000006 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 5.9142(13) 5.9121(14) 5.9124(11) 59.96(2) 89.933(17) 59.98(2) V = 146.13(5) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) UB - matrix: -0.069818 0.031400 0.088871 ( 0.000020 0.000033 0.000027 ) -0.068966 -0.065428 -0.010108 ( 0.000017 0.000028 0.000022 ) 0.109166 -0.153001 0.116341 ( 0.000018 0.000029 0.000024 ) M - matrix: 0.021548 -0.014382 0.007193 ( 0.000005 0.000005 0.000004 ) -0.014382 0.028676 -0.014348 ( 0.000005 0.000010 0.000006 ) 0.007193 -0.014348 0.021535 ( 0.000004 0.000006 0.000007 ) unit cell: 5.9243(14) 5.9289(14) 5.9199(13) 60.02(2) 89.986(19) 59.91(2) V = 146.90(5) OTKP changes: 452 1 1 1 OTKP changes: 452 1 1 1 OTKP changes: 452 1 1 1 UB - matrix: -0.069946 0.031440 0.088980 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.069946 0.031440 0.088980 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* UB - matrix: -0.069946 0.031440 0.088980 ( 0.000020 0.000032 0.000026 ) -0.069116 -0.065545 -0.010286 ( 0.000016 0.000027 0.000022 ) 0.109201 -0.153431 0.116531 ( 0.000015 0.000025 0.000021 ) M - matrix: 0.021594 -0.014424 0.007212 ( 0.000005 0.000005 0.000004 ) -0.014424 0.028826 -0.014408 ( 0.000005 0.000009 0.000005 ) 0.007212 -0.014408 0.021603 ( 0.000004 0.000005 0.000007 ) UB fit with 452 obs out of 452 (total:452,skipped:0) (100.00%) unit cell: 5.9156(14) 5.9109(13) 5.9105(13) 60.02(2) 90.012(18) 59.96(2) V = 146.07(5) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" PROFFIT INFO: Final refinement of average UB and unit cell UB - matrix: -0.069980 0.031127 0.088929 ( 0.000011 0.000013 0.000012 ) -0.068795 -0.065790 -0.010437 ( 0.000011 0.000014 0.000012 ) 0.109164 -0.153105 0.116431 ( 0.000009 0.000010 0.000009 ) M - matrix: 0.021547 -0.014366 0.007205 ( 0.000003 0.000002 0.000002 ) -0.014366 0.028738 -0.014371 ( 0.000002 0.000004 0.000002 ) 0.007205 -0.014371 0.021574 ( 0.000002 0.000002 0.000003 ) UB fit with 2250 obs out of 2250 (total:2250,skipped:0) (100.00%) unit cell: 5.9179(7) 5.9142(7) 5.9136(6) 60.046(12) 90.083(9) 60.035(13) V = 146.43(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 65 reflections under beam stop or inside a detector rejection region 18 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof 3047 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:34:03 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: P-lattice Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) PROFFIT INFO: signal sum: min=235.0000 max=20917466.0000 PROFFIT INFO: signal sum lp corr: min=469.1946 max=2977072.3592 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=750.7114 max=4763315.5000 PROFFIT INFO: sig(Inet): min=120.4339 max=47821.4375 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 33 149 318 624 700 1246 2040 2795 3047 Percent 0.0 0.0 1.1 4.9 10.4 20.5 23.0 40.9 67.0 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4763316- 1126874 304 1857498.68 122.08 100.00 1120714- 632191 304 856435.52 102.98 100.00 631660- 267498 304 418572.05 94.92 100.00 267414- 170043 304 203632.41 70.39 100.00 170007- 120782 304 145592.14 51.27 100.00 120556- 94182 304 106661.38 36.29 100.00 94162- 67231 304 81543.65 29.59 100.00 67065- 5692 304 38005.16 19.24 100.00 5683- 2972 304 3973.96 5.40 97.04 2970- 751 311 2128.02 3.72 54.98 ------------------------------------------------------------------------------------ 4763316- 751 3047 370555.94 53.47 95.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 304 625649.34 86.38 99.34 1.41- 1.05 304 603789.88 69.32 97.70 1.05- 0.92 304 450376.66 61.40 98.36 0.92- 0.82 304 325282.45 51.60 94.08 0.82- 0.74 304 429747.53 57.72 96.05 0.74- 0.67 304 360738.55 55.89 96.38 0.67- 0.61 304 202947.02 37.59 93.75 0.61- 0.56 304 295310.60 45.00 92.11 0.56- 0.51 304 226837.62 37.94 90.46 0.51- 0.40 311 189059.01 32.38 92.93 ------------------------------------------------------------------------------------ 5.26- 0.40 3047 370555.94 53.47 95.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:34:03 2018 Sorting 3047 observations 295 unique observations with > 7.00 F2/sig(F2) 3047 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 98 519 Total number of frames 519 Maximum number of 295 frame scales suggested for reliable scaling Glued frame scales: 2 frame = 1 scale 3047 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 2446 observations > 7.00 F2/sig(F2) 2446 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 2446 removed 24 = 2422, unique = 284) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2422 observations in 5 runs Run # start # end # total # 1 0 54 55 2 0 49 105 3 0 53 159 4 0 53 213 5 0 49 263 Total number of frames 263 284 unique data precomputed (should be 284) 284 unique data with 2422 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 8.5 (Out of 2422 removed 0 = 2422, unique = 284) 284 unique data precomputed (should be 284) 284 unique data with 2422 observations RMS deviation of equivalent data = 0.73699 Rint = 0.69842 14 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.67905, wR= 3.49972 Trying model 1 (ne=2, no=0)... Results: Rint= 0.68775, wR= 2.85658, Acormin=0.137, Acormax=1.981, Acor_av=0.839 F test: Probability=0.000, F= 0.973 Trying model 2 (ne=2, no=1)... Results: Rint= 0.73046, wR= 2.84989, Acormin=-0.166, Acormax=1.876, Acor_av=0.737 F test: Probability=0.000, F= 0.861 Trying model 3 (ne=4, no=0)... Results: Rint= 0.73164, wR= 2.44968, Acormin=-0.172, Acormax=2.319, Acor_av=0.699 F test: Probability=0.000, F= 0.856 Trying model 4 (ne=4, no=1)... Results: Rint= 0.78166, wR= 2.39147, Acormin=-0.523, Acormax=1.923, Acor_av=0.599 F test: Probability=0.000, F= 0.749 Trying model 5 (ne=4, no=3)... Results: Rint= 0.78859, wR= 2.47354, Acormin=-0.727, Acormax=1.960, Acor_av=0.537 F test: Probability=0.000, F= 0.733 Trying model 6 (ne=6, no=0)... Results: Rint= 0.75195, wR= 2.39680, Acormin=-0.324, Acormax=2.621, Acor_av=0.632 F test: Probability=0.000, F= 0.805 Trying model 7 (ne=6, no=1)... Results: Rint= 0.79914, wR= 2.39105, Acormin=-0.562, Acormax=2.252, Acor_av=0.523 F test: Probability=0.000, F= 0.712 Trying model 8 (ne=6, no=3)... Results: Rint= 0.81528, wR= 2.43366, Acormin=-0.994, Acormax=2.099, Acor_av=0.461 F test: Probability=0.000, F= 0.682 Trying model 9 (ne=6, no=5)... Results: Rint= 0.83943, wR= 2.47644, Acormin=-1.103, Acormax=2.237, Acor_av=0.380 F test: Probability=0.000, F= 0.640 Trying model 10 (ne=8, no=0)... Results: Rint= 0.82610, wR= 2.16305, Acormin=-0.711, Acormax=2.176, Acor_av=0.452 F test: Probability=0.000, F= 0.662 Trying model 11 (ne=8, no=1)... Results: Rint= 0.89937, wR= 1.82706, Acormin=-0.943, Acormax=1.488, Acor_av=0.250 F test: Probability=0.000, F= 0.557 Trying model 12 (ne=8, no=3)... Results: Rint= 0.98809, wR= 1.55040, Acormin=-0.047, Acormax=0.068, Acor_av=0.001 F test: Probability=0.000, F= 0.460 Trying model 13 (ne=8, no=5)... Results: Rint= 0.98958, wR= 1.58018, Acormin=-0.054, Acormax=0.068, Acor_av=0.002 F test: Probability=0.000, F= 0.456 Trying model 14 (ne=8, no=7)... Results: Rint= 1.00377, wR= 1.66901, Acormin=-0.050, Acormax=0.065, Acor_av=0.001 F test: Probability=0.000, F= 0.440 Choosing minimum absorption correction model (ne=2, no=0) due to no significant data quality improvement using higher order models Combined refinement in use Rint: 0.86663 There are 263 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 267 pars with 35778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.73699 Using Levenberg-Marquardt: 0.00010 New wR= 0.71484 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.69842 with corrections 0.67665 Rint for all data: 0.86663 with corrections 0.85122 15 observations identified as outliers and rejected Cycle 2 wR= 0.68949 Using Levenberg-Marquardt: 0.00001 New wR= 0.68726 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.67804 with corrections 0.66084 Rint for all data: 0.86663 with corrections 0.85701 11 observations identified as outliers and rejected Cycle 3 wR= 0.66888 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.66481 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66812 with corrections 0.65067 Rint for all data: 0.86663 with corrections 0.85655 10 observations identified as outliers and rejected Cycle 4 wR= 0.64222 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.64076 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66370 with corrections 0.66131 Rint for all data: 0.86663 with corrections 0.86584 3 observations identified as outliers and rejected Cycle 5 wR= 0.63781 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.63103 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.66142 with corrections 0.66100 Rint for all data: 0.86663 with corrections 0.86556 5 observations identified as outliers and rejected Final wR= 0.63103 Final frame scales: Min= 1.0000 Max= 7.1047 Final absorption correction factors: Amin= 0.2269 Amax= 1.7574 Frame scales outside specified range! Trying one more time with different frame scales initialization There are 263 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 267 pars with 35778 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.84560 Using Levenberg-Marquardt: 0.00010 New wR= 0.84840 Using Levenberg-Marquardt: 0.00100 New wR= 0.81135 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65895 with corrections 1.33001 Rint for all data: 0.86663 with corrections 1.39125 2 observations identified as outliers and rejected Cycle 2 wR= 0.80180 Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 New wR= 0.68786 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65840 with corrections 1.70093 Rint for all data: 0.86663 with corrections 1.73262 3 observations identified as outliers and rejected Cycle 3 wR= 0.68277 Using Levenberg-Marquardt: 0.01000 New wR= 0.63118 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65790 with corrections 1.22784 Rint for all data: 0.86663 with corrections 1.29375 3 observations identified as outliers and rejected Cycle 4 wR= 0.62928 Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.62112 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65722 with corrections 0.72921 Rint for all data: 0.86663 with corrections 0.90742 1 observations identified as outliers and rejected Cycle 5 wR= 0.62030 Using Levenberg-Marquardt: 0.10000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 1.00000 New wR= 0.61516 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.65708 with corrections 0.68859 Rint for all data: 0.86663 with corrections 0.88261 2 observations identified as outliers and rejected Final wR= 0.61516 Final frame scales: Min= 0.4310 Max= 5.7556 Final absorption correction factors: Amin= 0.1013 Amax= 1.7974 Frame scales outside specified range! Trying one more time after skipping bad frame scales There are 251 active scales (one needs to be fixed) Refinement control: frame scale #167 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 2, max odd order: 0 (5 parameters) Refinement control: 255 pars with 32640 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.74975 Using Levenberg-Marquardt: 0.00010 New wR= 0.63414 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65624 with corrections 0.66004 Rint for all data: 0.86663 with corrections 0.87000 8 observations identified as outliers and rejected Cycle 2 wR= 0.59774 Using Levenberg-Marquardt: 0.00001 New wR= 0.58190 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65379 with corrections 0.63013 Rint for all data: 0.86663 with corrections 0.85370 6 observations identified as outliers and rejected Cycle 3 wR= 0.56452 Using Levenberg-Marquardt: 0.00000 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00001 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00010 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.00100 Matrix singular! Adjusting LS parameters... Using Levenberg-Marquardt: 0.01000 New wR= 0.56432 There are 1 clusters with unrefined scales (size 12-12) Rint for refined data: 0.65223 with corrections 0.62804 Rint for all data: 0.86663 with corrections 0.85497 Final wR= 0.56432 Final frame scales: Min= 0.8260 Max= 2.7311 Final absorption correction factors: Amin= 0.3341 Amax= 1.4468 2 frames rejected due to unexpectedly low intensity PROFFIT INFO: Inet (after scale3 abspack): min=661.3864 max=5897814.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=120.8710 max=65563.5313 PROFFIT INFO: 14 observations on 'bad frames' rejected ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/5 frame:1/109 3033 reflections read from tmp file 2265 reflections are rejected (2203 as outliers, 62 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 80 63 33 22 10 9 2 3 1 Initial Chi^2= 0.66332 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.92629 Current error model SIG(F2)^2 = 298.22*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 276.23*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 276.23*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5897814- 1093330 303 1842005.24 88.07 100.00 1090994- 573600 303 805039.55 43.10 100.00 569676- 256013 303 391301.72 38.97 100.00 255759- 159067 303 200299.85 29.91 100.00 158829- 120935 303 138912.64 20.17 100.00 120806- 87374 303 103362.24 15.16 100.00 87343- 61300 303 73166.72 11.85 100.00 61202- 5504 303 35850.63 8.61 92.41 5477- 2606 303 3620.81 3.02 33.00 2603- 661 306 2017.75 2.44 16.34 ------------------------------------------------------------------------------------ 5897814- 661 3033 359204.06 26.11 84.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 303 735690.68 57.33 95.05 1.41- 1.05 303 592505.30 39.67 93.07 1.05- 0.92 303 447572.39 30.85 89.44 0.92- 0.82 303 315797.02 22.89 79.54 0.82- 0.74 303 422199.27 25.91 86.47 0.74- 0.67 303 331446.73 22.70 84.82 0.67- 0.61 303 177967.42 15.04 77.89 0.61- 0.56 303 249827.38 18.10 78.22 0.56- 0.51 303 184380.59 15.38 78.55 0.51- 0.40 306 136855.33 13.32 78.10 ------------------------------------------------------------------------------------ 5.26- 0.40 3033 359204.06 26.11 84.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5.26- 1.41 303 735690.68 57.33 95.05 5.26- 1.05 606 664097.99 48.50 94.06 5.26- 0.92 909 591922.79 42.62 92.52 5.26- 0.82 1212 522891.35 37.69 89.27 5.26- 0.74 1515 502752.93 35.33 88.71 5.26- 0.67 1818 474201.90 33.23 88.06 5.26- 0.61 2121 431882.69 30.63 86.61 5.26- 0.56 2424 409125.77 29.06 85.56 5.26- 0.51 2727 384154.09 27.54 84.78 5.26- 0.40 3033 359204.06 26.11 84.11 ------------------------------------------------------------------------------------ 5.26- 0.40 3033 359204.06 26.11 84.11 Scale applied to data: s=0.169554 (maximum obs:5897814.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.852; Rsigma 0.025: data 3033 -> merged 319 With outlier rejection... Rint 0.798; Rsigma 0.025: data 2906 -> merged 319 Rejected total: 127, method kkm 113, method Blessing 14 Completeness direct cell (a, b, c) = (5.271, 5.271, 5.271), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.404248, 5.270745 completeness table (Laue group: Pm-3, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.46 15 15 14.67 100.00 220 1.46 - 1.12 15 15 21.80 100.00 327 1.08 - 0.96 15 15 18.13 100.00 272 0.96 - 0.86 15 15 16.67 100.00 250 0.86 - 0.79 15 15 14.53 100.00 218 0.79 - 0.73 15 15 12.73 100.00 191 0.73 - 0.69 15 15 11.80 100.00 177 0.69 - 0.65 15 15 12.13 100.00 182 0.65 - 0.63 15 15 7.87 100.00 118 0.63 - 0.60 21 21 8.62 100.00 181 --------------------------------------------------------------- 5.92 - 0.60 156 156 13.69 100.00 2136 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:34:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917906 5.914182 5.913572 60.0464 90.0833 60.0351 2905 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1461 1523 1454 1463 2219 1954 1924 2905 N (int>3sigma) = 0 1201 1523 1194 1219 1959 1650 1616 2438 Mean intensity = 0.0 54.3 24.5 54.3 55.5 44.1 60.2 57.9 58.5 Mean int/sigma = 0.0 24.9 21.4 24.6 24.8 23.6 26.2 25.7 25.7 Lattice type: P chosen Volume: 146.43 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.914 90.06 119.94 119.95 Niggli form: a.a = 34.970 b.b = 34.978 c.c = 34.980 b.c = -0.034 a.c = -17.457 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.089 CUBIC F-lattice R(int) = 0.175 [ 2749] Vol = 585.7 Cell: 8.368 8.372 8.360 90.04 90.00 90.01 Volume: 585.70 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 2470] Vol = 439.3 Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.28 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.169 [ 788] Vol = 439.3 Trigonal Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.28 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.018 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.9 Cell: 5.919 5.918 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.048 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.9 Cell: 5.918 5.919 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 2452] Vol = 292.9 Cell: 5.918 5.919 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.148 [ 2451] Vol = 292.9 Cell: 5.914 8.368 5.918 89.99 89.92 89.99 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.137 [ 2113] Vol = 292.9 Cell: 5.919 5.918 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.060 MONOCLINIC I-lattice R(int) = 0.139 [ 2114] Vol = 292.9 Cell: 5.914 5.918 8.368 90.01 90.01 89.92 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.007 MONOCLINIC I-lattice R(int) = 0.137 [ 2135] Vol = 292.9 Cell: 5.914 8.368 5.918 89.99 90.08 90.01 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.036 MONOCLINIC I-lattice R(int) = 0.131 [ 2112] Vol = 292.9 Cell: 5.918 5.914 8.368 89.99 90.01 90.08 Volume: 292.85 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.156 [ 2120] Vol = 292.9 Cell: 10.247 5.914 5.914 90.06 125.21 89.95 Volume: 292.85 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.116 [ 1528] Vol = 146.4 Cell: 5.914 5.914 5.914 90.06 119.94 119.95 Volume: 146.43 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1523 0 1956 1946 2905 N (int>3sigma) = 0 0 0 0 1523 0 1648 1649 2438 Mean intensity = 0.0 0.0 0.0 0.0 24.5 0.0 57.9 58.5 58.5 Mean int/sigma = 0.0 0.0 0.0 0.0 21.4 0.0 25.6 25.8 25.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.143 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 217 661 N I>3s 28 28 103 661 0.8 0.8 0.6 29.2 6.3 6.3 3.5 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 2552 Fd-3m 1 1 227 C N N N N 37 2284 0.176 2590 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368141 8.372198 8.360035 90.0420 89.9976 90.0112 ZERR 1.00 0.003434 0.001602 0.000272 0.0011 0.0115 0.0014 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Pm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3075674- 584939 527 503 31 16.2 888920.79 53.61 0.701 0.684 584759- 444841 376 369 31 11.9 508372.43 32.14 0.944 0.873 421058- 334253 333 329 31 10.6 376694.10 28.94 0.902 0.875 333121- 271972 345 335 31 10.8 287249.71 23.06 0.936 1.008 267922- 201996 280 260 31 8.4 190466.68 16.39 0.922 0.972 201840- 151848 327 308 31 9.9 160326.94 18.72 0.741 0.941 148934- 91254 294 273 31 8.8 93812.79 13.53 0.604 0.629 89836- 61690 218 210 31 6.8 74976.86 12.00 0.497 0.324 61119- 47456 170 165 31 5.3 54325.94 9.60 0.496 0.421 47403- 1793 163 154 40 3.9 30319.09 6.50 0.604 0.540 ------------------------------------------------------------------------------------------- 3075674- 1793 3033 2906 319 9.1 347133.03 25.77 0.798 0.797 Statistics vs resolution - point group symmetry: Pm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.08 596 574 31 18.5 651663.38 48.33 0.788 0.849 0.015 1.05-0.83 539 527 32 16.5 403292.11 28.04 0.904 1.056 0.023 0.82-0.72 438 430 32 13.4 344068.87 23.30 0.787 0.863 0.028 0.72-0.65 373 358 32 11.2 253033.32 19.48 0.828 0.861 0.033 0.64-0.60 286 272 31 8.8 248097.08 18.04 0.821 0.908 0.035 0.59-0.56 232 218 31 7.0 156655.24 13.85 0.661 0.584 0.045 0.56-0.52 197 182 32 5.7 206714.04 16.91 0.646 0.598 0.041 0.52-0.49 166 156 31 5.0 122799.83 11.91 0.697 0.636 0.050 0.49-0.46 114 107 31 3.5 152739.28 14.20 0.491 0.408 0.045 0.46-0.40 92 82 36 2.3 108393.07 12.34 0.296 0.209 0.053 ------------------------------------------------------------------------------------------------------ inf-0.40 3033 2906 319 9.1 347133.03 25.77 0.798 0.797 0.025 inf-0.60 2206 2137 156 13.7 415874.56 29.94 0.823 0.904 0.022 Statistics vs resolution (taking redundancy into account) - point group symmetry: Pm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.08 574 31 31 100.0 18.5 651663.38 228.74 0.788 0.004 1.05-0.83 527 32 32 100.0 16.5 403292.11 137.03 0.904 0.008 0.82-0.72 430 32 32 100.0 13.4 344068.87 100.35 0.787 0.011 0.72-0.65 358 32 32 100.0 11.2 253033.32 82.05 0.828 0.014 0.64-0.60 272 31 31 100.0 8.8 248097.08 68.33 0.821 0.016 0.59-0.56 218 34 31 91.2 7.0 156655.24 46.42 0.661 0.022 0.56-0.52 182 35 32 91.4 5.7 206714.04 50.56 0.646 0.021 0.52-0.49 156 44 31 70.5 5.0 122799.83 32.72 0.697 0.027 0.49-0.46 107 57 31 54.4 3.5 152739.28 31.79 0.491 0.027 0.46-0.40 82 136 36 26.5 2.3 108393.07 20.79 0.296 0.033 -------------------------------------------------------------------------------------------- inf-0.40 2906 464 319 68.8 9.1 347133.03 111.55 0.798 0.013 inf-0.60 2137 156 156 100.0 13.7 415874.56 137.18 0.823 0.009 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 RRPPROF to HKL transformation matrix: -1.0 2.0 -1.0 1.0 0.0 -1.0 -1.0 0.0 -1.0 No constraint UB - matrix: 0.015564 -0.079454 -0.025038 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029179 0.072511 ( 0.000007 0.000007 0.000006 ) -0.076552 -0.003634 -0.036245 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007185 0.000001 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007177 0.000005 ( 0.000001 0.000001 0.000001 ) -0.000000 0.000005 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: 0.015564 -0.079454 -0.025038 ( 0.000007 0.000007 0.000006 ) -0.032895 -0.029179 0.072511 ( 0.000007 0.000007 0.000006 ) -0.076552 -0.003634 -0.036245 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3682(5) 8.3723(7) 8.3601(6) 90.042(6) 89.998(5) 90.011(6) V = 585.71(7) unit cell: 8.36685(18) 8.36685(18) 8.36685(18) 90.0 90.0 90.0 V = 585.71(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.772) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.772) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.911) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.772) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.772) PROFFIT INFO: signal sum: min=235.0000 max=20917466.0000 PROFFIT INFO: signal sum lp corr: min=469.1946 max=2977072.3592 PROFFIT INFO: background sum: min=600.0000 max=25985.0000 PROFFIT INFO: background sum sig2: min=534.0000 max=12347.0000 PROFFIT INFO: num of signal pixels: min=48 max=556 PROFFIT INFO: Inet: min=750.7114 max=4763315.5000 PROFFIT INFO: sig(Inet): min=120.4339 max=47821.4375 PROFFIT INFO: Inet/sig(Inet): min=0.95 max=249.38 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 66 298 636 1248 1400 2492 4080 5590 6094 Percent 0.0 0.0 1.1 4.9 10.4 20.5 23.0 40.9 67.0 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3047 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3047 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4763316- 1126874 304 1857498.68 122.08 100.00 1120714- 632191 304 856435.52 102.98 100.00 631660- 267498 304 418572.05 94.92 100.00 267414- 170043 304 203632.41 70.39 100.00 170007- 120782 304 145592.14 51.27 100.00 120556- 94182 304 106661.38 36.29 100.00 94162- 67231 304 81543.65 29.59 100.00 67065- 5692 304 38005.16 19.24 100.00 5683- 2972 304 3973.96 5.40 97.04 2970- 751 311 2128.02 3.72 54.98 ------------------------------------------------------------------------------------ 4763316- 751 3047 370555.94 53.47 95.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 732043.22 93.49 100.00 1.41- 1.12 304 629551.94 63.27 99.34 1.12- 0.96 304 481167.92 70.27 97.70 0.96- 0.88 304 357398.15 60.14 94.74 0.88- 0.81 304 454294.56 68.89 99.34 0.81- 0.73 304 246718.65 41.11 95.72 0.73- 0.71 304 174247.29 33.81 87.17 0.71- 0.65 304 323096.04 48.53 95.07 0.65- 0.62 304 157006.42 27.68 87.17 0.62- 0.58 311 154998.73 28.13 94.86 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 370555.94 53.47 95.11 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:34:04 2018 Sorting 3047 observations 85 unique observations with > 7.00 F2/sig(F2) 3047 observations in 5 runs Run # start # end # total # 1 0 108 109 2 1 98 207 3 0 106 314 4 1 107 421 5 1 98 519 Total number of frames 519 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3047 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 2446 observations > 7.00 F2/sig(F2) 2446 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 26.3 (Out of 2446 removed 3 = 2443, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2443 observations in 5 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 Total number of frames 78 93 unique data precomputed (should be 93) 93 unique data with 2443 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.3 (Out of 2443 removed 0 = 2443, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2443 observations RMS deviation of equivalent data = 0.26313 Rint = 0.18815 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18045, wR= 0.27577 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13646, wR= 0.17924, Acormin=0.601, Acormax=1.405, Acor_av=0.977 F test: Probability=1.000, F= 1.745 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11334, wR= 0.14643, Acormin=0.559, Acormax=1.478, Acor_av=0.913 F test: Probability=1.000, F= 1.448 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10724, wR= 0.14571, Acormin=0.581, Acormax=1.552, Acor_av=0.942 F test: Probability=0.995, F= 1.114 Trying model 4 (ne=4, no=1)... Results: Rint= 0.08838, wR= 0.11935, Acormin=0.499, Acormax=1.573, Acor_av=0.878 F test: Probability=1.000, F= 1.471 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07680, wR= 0.10881, Acormin=0.473, Acormax=1.602, Acor_av=0.888 F test: Probability=1.000, F= 1.320 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10002, wR= 0.13854, Acormin=0.592, Acormax=1.613, Acor_av=0.950 F test: Probability=0.000, F= 0.589 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08187, wR= 0.11318, Acormin=0.481, Acormax=1.614, Acor_av=0.884 F test: Probability=0.000, F= 0.878 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07366, wR= 0.10384, Acormin=0.456, Acormax=1.628, Acor_av=0.894 F test: Probability=0.969, F= 1.081 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07214, wR= 0.10159, Acormin=0.320, Acormax=1.425, Acor_av=0.778 F test: Probability=0.812, F= 1.038 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09725, wR= 0.13467, Acormin=0.554, Acormax=1.597, Acor_av=0.922 F test: Probability=0.000, F= 0.572 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08140, wR= 0.11149, Acormin=0.459, Acormax=1.499, Acor_av=0.805 F test: Probability=0.000, F= 0.815 Trying model 12 (ne=8, no=3)... Results: Rint= 0.07853, wR= 0.10610, Acormin=0.110, Acormax=0.398, Acor_av=0.215 F test: Probability=0.000, F= 0.873 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07184, wR= 0.09778, Acormin=0.120, Acormax=0.447, Acor_av=0.242 F test: Probability=0.817, F= 1.039 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06290, wR= 0.08919, Acormin=0.159, Acormax=0.499, Acor_av=0.260 F test: Probability=1.000, F= 1.346 Final absorption model (ne=6, no=3): Rint= 0.07366, Acormin=0.456, Acormax=1.628, Acor_av=0.894 Combined refinement in use Rint: 0.18826 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 114 pars with 6555 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26313 Using Levenberg-Marquardt: 0.00010 New wR= 0.06328 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18815 with corrections 0.05022 Rint for all data: 0.18826 with corrections 0.05043 0 observations identified as outliers and rejected Cycle 2 wR= 0.06328 Using Levenberg-Marquardt: 0.00001 New wR= 0.05849 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18815 with corrections 0.04600 Rint for all data: 0.18826 with corrections 0.04623 0 observations identified as outliers and rejected Cycle 3 wR= 0.05849 Using Levenberg-Marquardt: 0.00000 New wR= 0.05750 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18815 with corrections 0.04510 Rint for all data: 0.18826 with corrections 0.04532 0 observations identified as outliers and rejected Cycle 4 wR= 0.05750 Using Levenberg-Marquardt: 0.00000 New wR= 0.05702 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18815 with corrections 0.04462 Rint for all data: 0.18826 with corrections 0.04484 0 observations identified as outliers and rejected Cycle 5 wR= 0.05702 Using Levenberg-Marquardt: 0.00000 New wR= 0.05670 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18815 with corrections 0.04432 Rint for all data: 0.18826 with corrections 0.04454 0 observations identified as outliers and rejected Final wR= 0.05670 Final frame scales: Min= 0.7423 Max= 1.2869 Final absorption correction factors: Amin= 0.4866 Amax= 1.3482 PROFFIT INFO: Inet (after scale3 abspack): min=795.2933 max=4679920.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=108.3684 max=52477.0742 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/5 frame:1/109 3047 reflections read from tmp file 604 reflections are rejected (604 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 4 1 3 0 6 4 85 Initial Chi^2= 0.39675 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.98498 Current error model SIG(F2)^2 = 166.38*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 330.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 330.26*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4679921- 1096891 304 1753839.06 81.55 100.00 1096316- 609820 304 815337.80 36.75 100.00 609580- 257673 304 405010.14 38.28 100.00 257401- 155195 304 192817.42 27.10 100.00 155179- 125629 304 140008.18 18.39 100.00 125589- 87681 304 102927.43 13.09 100.00 87583- 68965 304 78575.88 10.87 100.00 68949- 4950 304 40047.79 7.60 87.17 4935- 2751 304 3632.92 2.76 19.74 2751- 795 311 2146.96 2.28 10.93 ------------------------------------------------------------------------------------ 4679921- 795 3047 352627.33 23.82 81.62 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 734421.35 57.73 98.03 1.41- 1.12 304 612269.88 37.56 87.50 1.12- 0.96 304 440697.30 29.49 83.55 0.96- 0.88 304 335761.68 22.20 83.22 0.88- 0.81 304 428673.19 25.02 90.13 0.81- 0.73 304 228865.11 15.22 69.08 0.73- 0.71 304 162320.07 12.59 75.66 0.71- 0.65 304 299708.54 17.71 90.79 0.65- 0.62 304 146362.63 10.41 68.09 0.62- 0.58 311 142042.55 10.55 70.42 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 352627.33 23.82 81.62 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 304 734421.35 57.73 98.03 4.82- 1.12 608 673345.62 47.64 92.76 4.82- 0.96 912 595796.18 41.59 89.69 4.82- 0.88 1216 530787.55 36.74 88.08 4.82- 0.81 1520 510364.68 34.40 88.49 4.82- 0.73 1824 463448.09 31.20 85.25 4.82- 0.71 2128 420429.80 28.54 83.88 4.82- 0.65 2432 405339.64 27.19 84.75 4.82- 0.62 2736 376564.42 25.32 82.89 4.82- 0.58 3047 352627.33 23.82 81.62 ------------------------------------------------------------------------------------ 4.82- 0.58 3047 352627.33 23.82 81.62 Scale applied to data: s=0.213679 (maximum obs:4679920.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.045; Rsigma 0.027: data 3047 -> merged 110 With outlier rejection... Rint 0.042; Rsigma 0.028: data 3030 -> merged 110 Rejected total: 17, method kkm 9, method Blessing 8 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585796, 4.830600 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 5.92 - 1.71 10 10 17.60 100.00 176 1.61 - 1.21 10 10 27.60 100.00 276 1.17 - 1.01 10 10 36.00 100.00 360 0.99 - 0.89 10 10 35.30 100.00 353 0.88 - 0.81 10 10 34.00 100.00 340 0.81 - 0.74 10 10 29.30 100.00 293 0.73 - 0.71 10 10 32.20 100.00 322 0.70 - 0.66 10 10 27.30 100.00 273 0.66 - 0.64 10 10 24.90 100.00 249 0.63 - 0.60 10 10 24.10 100.00 241 --------------------------------------------------------------- 5.92 - 0.60 100 100 28.83 100.00 2883 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:34:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 5.917906 5.914182 5.913572 60.0464 90.0833 60.0351 2905 Reflections read from file xs1714a.hkl; mean (I/sigma) = 25.69 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 1461 1523 1454 1463 2219 1954 1924 2905 N (int>3sigma) = 0 1201 1523 1194 1219 1959 1650 1616 2438 Mean intensity = 0.0 54.3 24.5 54.3 55.5 44.1 60.2 57.9 58.5 Mean int/sigma = 0.0 24.9 21.4 24.6 24.8 23.6 26.2 25.7 25.7 Lattice type: P chosen Volume: 146.43 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Unitcell: 5.914 5.914 5.914 90.06 119.94 119.95 Niggli form: a.a = 34.970 b.b = 34.978 c.c = 34.980 b.c = -0.034 a.c = -17.457 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.089 CUBIC F-lattice R(int) = 0.175 [ 2749] Vol = 585.7 Cell: 8.368 8.372 8.360 90.04 90.00 90.01 Volume: 585.70 Matrix:-1.0000 2.0000 -1.0000 1.0000 0.0000 -1.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.168 [ 2470] Vol = 439.3 Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.28 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.079 RHOMBOHEDRAL R-lattice R(int) = 0.169 [ 788] Vol = 439.3 Trigonal Cell: 5.918 5.914 14.496 90.03 90.04 120.03 Volume: 439.28 Matrix: 0.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -3.0000 2.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.018 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.9 Cell: 5.919 5.918 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 1.0000 -1.0000 0.0000 0.0000 1.0000 -1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.048 TETRAGONAL I-lattice R(int) = 0.149 [ 2502] Vol = 292.9 Cell: 5.918 5.919 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix: 0.0000 1.0000 -1.0000 1.0000 -1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.023 ORTHORHOMBIC I-lattice R(int) = 0.152 [ 2452] Vol = 292.9 Cell: 5.918 5.919 8.360 89.97 89.97 89.97 Volume: 292.85 Matrix: 0.0000 -1.0000 1.0000 -1.0000 1.0000 0.0000 -1.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.036 ORTHORHOMBIC I-lattice R(int) = 0.148 [ 2451] Vol = 292.9 Cell: 5.914 8.368 5.918 89.99 89.92 89.99 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 2.0000 -1.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.137 [ 2113] Vol = 292.9 Cell: 5.919 5.918 8.360 90.03 90.03 89.97 Volume: 292.85 Matrix:-1.0000 1.0000 0.0000 0.0000 -1.0000 1.0000 1.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.060 MONOCLINIC I-lattice R(int) = 0.139 [ 2114] Vol = 292.9 Cell: 5.914 5.918 8.368 90.01 90.01 89.92 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.007 MONOCLINIC I-lattice R(int) = 0.137 [ 2135] Vol = 292.9 Cell: 5.914 8.368 5.918 89.99 90.08 90.01 Volume: 292.85 Matrix: 0.0000 0.0000 1.0000 1.0000 -2.0000 1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.036 MONOCLINIC I-lattice R(int) = 0.131 [ 2112] Vol = 292.9 Cell: 5.918 5.914 8.368 89.99 90.01 90.08 Volume: 292.85 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 -2.0000 1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.060 MONOCLINIC C-lattice R(int) = 0.156 [ 2120] Vol = 292.9 Cell: 10.247 5.914 5.914 90.06 125.21 89.95 Volume: 292.85 Matrix: 0.0000 1.0000 -2.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.116 [ 1528] Vol = 146.4 Cell: 5.914 5.914 5.914 90.06 119.94 119.95 Volume: 146.43 Matrix: 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 -1.0000 1.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1523 0 1956 1946 2905 N (int>3sigma) = 0 0 0 0 1523 0 1648 1649 2438 Mean intensity = 0.0 0.0 0.0 0.0 24.5 0.0 57.9 58.5 58.5 Mean int/sigma = 0.0 0.0 0.0 0.0 21.4 0.0 25.6 25.8 25.7 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.143 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 217 661 N I>3s 28 28 103 661 0.8 0.8 0.6 29.2 6.3 6.3 3.5 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.175 2552 Fd-3m 1 1 227 C N N N N 37 2284 0.176 2590 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=1.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.368141 8.372198 8.360035 90.0420 89.9976 90.0112 ZERR 1.00 0.003434 0.001602 0.000272 0.0011 0.0115 0.0014 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 11.00 10.00 1.00 1.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3966772- 518863 673 662 27 24.5 1189995.53 54.82 0.038 0.043 506327- 119808 906 902 27 33.4 213529.82 26.90 0.049 0.068 107606- 35321 753 753 27 27.9 79100.95 10.83 0.067 0.089 10224- 1822 715 713 29 24.6 3502.61 2.74 0.167 0.229 ------------------------------------------------------------------------------------------- 3966772- 1822 3047 3030 110 27.5 344040.04 23.32 0.042 0.050 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 765 750 27 27.8 596757.81 43.11 0.036 0.038 0.016 1.01-0.78 911 911 27 33.7 338062.93 21.41 0.033 0.041 0.028 0.78-0.65 797 796 27 29.5 249847.34 15.68 0.055 0.068 0.041 0.65-0.59 574 573 29 19.8 153611.06 11.07 0.078 0.094 0.058 ------------------------------------------------------------------------------------------------------ inf-0.59 3047 3030 110 27.5 344040.04 23.32 0.042 0.050 0.028 inf-0.60 2897 2881 99 29.1 356056.85 24.04 0.041 0.048 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 750 27 27 100.0 27.8 596757.81 232.57 0.036 0.003 1.01-0.78 911 27 27 100.0 33.7 338062.93 125.54 0.033 0.005 0.78-0.65 796 27 27 100.0 29.5 249847.34 87.97 0.055 0.009 0.65-0.59 573 29 29 100.0 19.8 153611.06 56.33 0.078 0.018 -------------------------------------------------------------------------------------------- inf-0.59 3030 110 110 100.0 27.5 344040.04 129.07 0.042 0.006 inf-0.60 2881 99 99 100.0 29.1 356056.85 133.49 0.041 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC FULLAUTOANALYSECONCURRENT Process information (Tue Mar 27 15:39:17 2018) ID: 2932; threads 39; handles 879; mem 523012.00 (1239492.00)kB; time: 1w 5d 0h 44m 47s MEMORY INFO: Memory PF:6.0, Ph:235.0, V:1210.0; MEMORY INFO: Process info - Handles: 880, Memory: PF:512.4,peak PF: 697.1, WS: 303.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) CRYSALIS auto analyse procedure 2005-2017 (version 1.0.2) AUTO INFO: Started at Tue Mar 27 15:39:17 2018 AUTO INFO: Experiment: D:\Data\xs1714a\xs1714a.run AUTO INFO: Clearing peak tables (hunting=200000 peaks,xyz=100000 peaks) MACHINE INFORMATION - GONIOMETER (RIGAKU) OXFORD DIFFRACTION/AGILENT TECHNOLOGIES KM4 XCALIBUR - ALPHA (DEG) 50.02178 BETA (DEG) -0.00611 - WAVELENGTH MO (ANG): A1 0.70930 A2 0.71359 B1 0.63229 - POLARISATION FACTOR 0.50000 - X-RAY BEAM ORIENTATION (DEG): X2 -0.00984 X3 0.00000 - BEAM PATH ABSORPTIONCOEFFICIENTS (MM-1): AIR 0.00013 BE 0.04736 - BE THICKNESS (MM): 0.50000 - SOFTWARE ZEROCORRECTION (DEG): OMEGA 0.00285 THETA -0.14800 KAPPA -0.13240 PHI 0.00000 DETECTOR 0.00000 - MACHINE OFFSETS (STEPS): OMEGA 0 THETA 0 KAPPA 0 PHI 0 DETECTOR 134439 - CCD DETECTOR ATLAS - CHIP: Kodak_KAF4320 B2 (2048x2048) 5629 - TAPER: Incom (B1,3620-2), ZOOM 2.005621 PIXELSIZE IN 1X1 BINNING (MM) 0.04813 - GAIN 90.00 (DOUBLE-CORRELATED-DIVIDE-BY-2 GAIN), IMAGE GAIN 90.00, ELECTRONS/ADU 2.10 - DETECTOR ROTATION (DEG): X1 0.74600 X2 -0.07600 X3 0.00000 - DETECTOR DISTANCE (MM): 53.00000 - DETECTOR ZERO (PIX, 1X1 BINNING): X 1028.28400 Y 1027.50900 - DETECTOR BINNING (PIX): X: 4 Y: 4 (XW: 2048, YW: 2048) - FLAT FIELD CORRECTION FILES: floodmo_a_101_calib_110512.ffiinffit floodcu_a_101_calib_110512.ffiinffit - GEOMETRIC CORRECTION FILE : a_101_020512.geo - GEOMETRIC CORRECTION STATUS: ALLOCATED:1, USED:1, GRIDX:255, GRIDY:255 - GEOMETRIC CORRECTION GRID LOADED: C:\Xcalibur\corrections\a_101\a_101_020512.geo - NO PIXEL DETECTOR CORRECTIONS! PROGRAM VERSION - PROGRAM RED 39.29c (release 19-06-2017) - (X)PAR FILE NAME xs1714a\xs1714a.par ******************************************************************************************************* Auto analyse stage: PEAK HUNTING (Tue Mar 27 15:39:17 2018) ******************************************************************************************************* CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -77.13 ph= 0.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.10 ka= -50.13 ph= 99.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 150.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= -90.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= -57.13 ph= -120.00 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.96 ka= 76.87 ph= 30.00 AUTO INFO: 7068 peaks in the peak location table 7068 peak locations are merged to 3244 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 3244 unindexed peaks to the CrysAlis peak table (3244 with profile info) ******************************************************************************************************* Auto analyse stage: CELL FINDING (Tue Mar 27 15:39:22 2018) ******************************************************************************************************* Instrument model: dd: 53.00, x0: 1028.28, y0: 1027.51, beam: -0.01, o0: 0.00, t0: -0.15, k0: -0.13 AUTO INFO: Dirax started... UM TTT - Duisenberg-like algorithm lattice finding - Rigaku Oxford Diffraction 2004-2017 (version: 1.5) UM TTT INFO: random number seed 1522179562! UM TTT INFO: Expected lattice sizes: min=2.000 max=120.000 UM TTT INFO: The intermediate cell results can be recalled from the UM TTTRINGBUFFER. All best cell results carry a consecutive solution number. The ring buffer is limited to 140 entries UM TTTSOLUTION 1: 1 418(sub) 2872(all), cF( 1,12) 8.38 8.38 8.39 90.05 90.07 90.01 pr: 147.15, r: 588.58 UM TTTSOLUTION 2: 2 348(sub) 2840(all), hP(12, 9) 5.92 5.92 14.52 90.00 90.06 119.94 pr: 441.60, r: 441.60 UM TTTSOLUTION 3: 3 384(sub) 2649(all), tI(15, 7) 8.38 8.38 16.76 89.92 89.96 90.00 pr: 588.97, r: 1177.93 UM TTTSOLUTION 4: 4 415(sub) 2286(all), hR( 9, 8) 5.93 5.93 29.02 90.00 90.07 120.09 pr: 294.15, r: 882.44 Peak table: 500(sub) 3244(all) Best cell: 418 indexed, Niggli cF( 1,12): 8.38 8.38 8.39 90.05 90.07 90.01 prim: 147.15, red: 588.58 UM TTTSOLUTION 1: 5 418(sub) 2872(all), cF( 1,12) 8.38 8.38 8.39 90.05 90.07 90.01 pr: 147.15, r: 588.58 UM TTTSOLUTION 2: 6 387(sub) 2841(all), hP(12, 9) 5.92 5.92 14.52 90.02 89.93 119.93 pr: 441.57, r: 441.57 UM TTTSOLUTION 3: 7 384(sub) 2649(all), tI(15, 7) 8.38 8.38 16.76 89.92 89.96 90.00 pr: 588.97, r: 1177.93 UM TTTSOLUTION 4: 8 388(sub) 2364(all), oI(42, 4) 5.93 8.39 29.62 90.03 90.05 90.06 pr: 736.18, r: 1472.37 UM TTTSOLUTION 5: 9 415(sub) 2286(all), hR( 9, 8) 5.93 5.93 29.02 90.00 90.07 120.09 pr: 294.15, r: 882.44 Peak table: 500(sub) 3244(all) Best cell: 418 indexed, Niggli cF( 1,12): 8.38 8.38 8.39 90.05 90.07 90.01 prim: 147.15, red: 588.58 UM TTTSOLUTION 1: 10 418(sub) 2872(all), cF( 1,12) 8.38 8.38 8.39 90.05 90.07 90.01 pr: 147.15, r: 588.58 UM TTTSOLUTION 2: 11 387(sub) 2841(all), hP(12, 9) 5.92 5.92 14.52 90.02 89.93 119.93 pr: 441.57, r: 441.57 UM TTTSOLUTION 3: 12 384(sub) 2649(all), tI(15, 7) 8.38 8.38 16.76 89.92 89.96 90.00 pr: 588.97, r: 1177.93 UM TTTSOLUTION 4: 13 388(sub) 2364(all), oI(42, 4) 5.93 8.39 29.62 90.03 90.05 90.06 pr: 736.18, r: 1472.37 UM TTTSOLUTION 5: 14 415(sub) 2286(all), hR( 9, 8) 5.93 5.93 29.02 90.00 90.07 120.09 pr: 294.15, r: 882.44 Peak table: 500(sub) 3244(all) Best cell: 418 indexed, Niggli cF( 1,12): 8.38 8.38 8.39 90.05 90.07 90.01 prim: 147.15, red: 588.58 UM TTTSOLUTION 1: 15 418(sub) 2872(all), cF( 1,12) 8.38 8.38 8.39 90.05 90.07 90.01 pr: 147.15, r: 588.58 UM TTTSOLUTION 2: 16 387(sub) 2841(all), hP(12, 9) 5.92 5.92 14.52 90.02 89.93 119.93 pr: 441.57, r: 441.57 UM TTTSOLUTION 3: 17 384(sub) 2649(all), tI(15, 7) 8.38 8.38 16.76 89.92 89.96 90.00 pr: 588.97, r: 1177.93 UM TTTSOLUTION 4: 18 388(sub) 2364(all), oI(42, 4) 5.93 8.39 29.62 90.03 90.05 90.06 pr: 736.18, r: 1472.37 UM TTTSOLUTION 5: 19 415(sub) 2286(all), hR( 9, 8) 5.93 5.93 29.02 90.00 90.07 120.09 pr: 294.15, r: 882.44 Peak table: 500(sub) 3244(all) Best cell: 418 indexed, Niggli cF( 1,12): 8.38 8.38 8.39 90.05 90.07 90.01 prim: 147.15, red: 588.58 Make subset: 0.00016 Make T-vectors: 0.39739 Make unit cell: 0.61476 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 3032 obs out of 3244 (total:3244,skipped:0) (93.46%) UB - matrix: 0.038674 0.069742 -0.158524 ( 0.000025 0.000024 0.000030 ) 0.134235 0.068635 -0.058154 ( 0.000025 0.000024 0.000030 ) 0.043961 -0.108992 -0.007270 ( 0.000021 0.000020 0.000025 ) M - matrix: 0.021447 0.007119 -0.014257 ( 0.000007 0.000005 0.000006 ) 0.007119 0.021454 -0.014255 ( 0.000005 0.000006 0.000006 ) -0.014257 -0.014255 0.028564 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9249(13) 5.9231(11) 5.9236(13) 60.08(2) 60.06(2) 90.018(16) V = 147.28(5) UB fit with 3033 obs out of 3244 (total:3244,skipped:0) (93.50%) UB - matrix: 0.038676 0.069739 -0.158523 ( 0.000025 0.000024 0.000030 ) 0.134233 0.068643 -0.058158 ( 0.000025 0.000024 0.000030 ) 0.043962 -0.108989 -0.007274 ( 0.000021 0.000020 0.000025 ) M - matrix: 0.021447 0.007120 -0.014258 ( 0.000007 0.000005 0.000006 ) 0.007120 0.021454 -0.014255 ( 0.000005 0.000006 0.000006 ) -0.014258 -0.014255 0.028565 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9251(13) 5.9231(11) 5.9236(13) 60.08(2) 60.06(2) 90.020(16) V = 147.28(5) UB fit with 3033 obs out of 3244 (total:3244,skipped:0) (93.50%) UB - matrix: 0.038677 0.069737 -0.158523 ( 0.000025 0.000024 0.000030 ) 0.134233 0.068642 -0.058158 ( 0.000025 0.000024 0.000030 ) 0.043962 -0.108989 -0.007274 ( 0.000021 0.000020 0.000025 ) M - matrix: 0.021447 0.007120 -0.014258 ( 0.000007 0.000005 0.000006 ) 0.007120 0.021454 -0.014254 ( 0.000005 0.000006 0.000006 ) -0.014258 -0.014254 0.028565 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9251(13) 5.9231(11) 5.9236(13) 60.08(2) 60.06(2) 90.020(16) V = 147.28(5) UM TTT INFO: No smaller volume found Primitive unit cell refinement UB fit with 3032 obs out of 3244 (total:3244,skipped:0) (93.46%) UB - matrix: 0.038674 0.069742 -0.158524 ( 0.000025 0.000024 0.000030 ) 0.134235 0.068635 -0.058154 ( 0.000025 0.000024 0.000030 ) 0.043961 -0.108992 -0.007270 ( 0.000021 0.000020 0.000025 ) M - matrix: 0.021447 0.007119 -0.014257 ( 0.000007 0.000005 0.000006 ) 0.007119 0.021454 -0.014255 ( 0.000005 0.000006 0.000006 ) -0.014257 -0.014255 0.028564 ( 0.000006 0.000006 0.000010 ) unit cell: 5.9249(13) 5.9231(11) 5.9236(13) 60.08(2) 60.06(2) 90.018(16) V = 147.28(5) No constraint UB - matrix: -0.025024 -0.079257 -0.015543 ( 0.000011 0.000012 0.000011 ) 0.072352 -0.029076 0.032807 ( 0.000011 0.000012 0.000011 ) -0.036175 -0.003636 0.076479 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.007170 0.000011 -0.000004 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007140 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000004 -0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025024 -0.079257 -0.015543 ( 0.000011 0.000012 0.000011 ) 0.072352 -0.029076 0.032807 ( 0.000011 0.000012 0.000011 ) -0.036175 -0.003636 0.076479 ( 0.000010 0.000010 0.000010 ) M - matrix: 0.007156 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007156 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007156 ( 0.000000 0.000000 0.000001 ) UB fit with 2867 obs out of 3244 (total:3244,skipped:0) (88.38%) unit cell: 8.3768(11) 8.3941(11) 8.3785(10) 89.999(10) 89.968(10) 90.089(11) V = 589.14(13) unit cell: 8.3831(3) 8.3831(3) 8.3831(3) 90.0 90.0 90.0 V = 589.14(4) AUTO INFO: Dirax ended... LAMBDA HALF REJECTION: Number of processed reflections: 1294 Number of skipped reflections, because of (potential) lambda half effect: 43 AUTO INFO: Dirax started... UM TTT - Duisenberg-like algorithm lattice finding - Rigaku Oxford Diffraction 2004-2017 (version: 1.5) UM TTT INFO: random number seed 1522179564! UM TTT INFO: Expected lattice sizes: min=2.000 max=120.000 UM TTT INFO: The intermediate cell results can be recalled from the UM TTTRINGBUFFER. All best cell results carry a consecutive solution number. The ring buffer is limited to 140 entries UM TTTSOLUTION 1: 1 440(sub) 2868(all), cF( 1,12) 8.37 8.39 8.38 89.94 89.93 90.12 pr: 147.16, r: 588.62 UM TTTSOLUTION 2: 2 400(sub) 2585(all), oI(42, 4) 5.92 8.38 17.80 90.01 90.07 89.99 pr: 441.56, r: 883.11 UM TTTSOLUTION 3: 3 415(sub) 2345(all), hR( 9, 8) 5.93 5.92 29.05 89.93 90.13 120.04 pr: 294.47, r: 883.41 Peak table: 500(sub) 3238(all) Best cell: 440 indexed, Niggli cF( 1,12): 8.37 8.39 8.38 89.94 89.93 90.12 prim: 147.16, red: 588.62 UM TTTSOLUTION 1: 4 440(sub) 2868(all), cF( 1,12) 8.37 8.39 8.38 89.94 89.93 90.12 pr: 147.16, r: 588.62 UM TTTSOLUTION 2: 5 400(sub) 2585(all), oI(42, 4) 5.92 8.38 17.80 90.01 90.07 89.99 pr: 441.56, r: 883.11 UM TTTSOLUTION 3: 6 407(sub) 2426(all), mC(39, 2) 19.64 5.93 10.27 90.16 100.08 89.90 pr: 589.10, r: 1178.19 UM TTTSOLUTION 4: 7 415(sub) 2345(all), hR( 9, 8) 5.93 5.92 29.05 89.93 90.13 120.04 pr: 294.47, r: 883.41 Peak table: 500(sub) 3238(all) Best cell: 440 indexed, Niggli cF( 1,12): 8.37 8.39 8.38 89.94 89.93 90.12 prim: 147.16, red: 588.62 UM TTTSOLUTION 1: 8 440(sub) 2868(all), cF( 1,12) 8.37 8.39 8.38 89.94 89.93 90.12 pr: 147.16, r: 588.62 UM TTTSOLUTION 2: 9 400(sub) 2585(all), oI(42, 4) 5.92 8.38 17.80 90.01 90.07 89.99 pr: 441.56, r: 883.11 UM TTTSOLUTION 3: 10 407(sub) 2426(all), mC(39, 2) 19.64 5.93 10.27 90.16 100.08 89.90 pr: 589.10, r: 1178.19 UM TTTSOLUTION 4: 11 415(sub) 2345(all), hR( 9, 8) 5.93 5.92 29.05 89.93 90.13 120.04 pr: 294.47, r: 883.41 Peak table: 500(sub) 3238(all) Best cell: 440 indexed, Niggli cF( 1,12): 8.37 8.39 8.38 89.94 89.93 90.12 prim: 147.16, red: 588.62 UM TTTSOLUTION 1: 12 440(sub) 2868(all), cF( 1,12) 8.37 8.39 8.38 89.94 89.93 90.12 pr: 147.16, r: 588.62 UM TTTSOLUTION 2: 13 400(sub) 2585(all), oI(42, 4) 5.92 8.38 17.80 90.01 90.07 89.99 pr: 441.56, r: 883.11 UM TTTSOLUTION 3: 14 407(sub) 2426(all), mC(39, 2) 19.64 5.93 10.27 90.16 100.08 89.90 pr: 589.10, r: 1178.19 UM TTTSOLUTION 4: 15 415(sub) 2345(all), hR( 9, 8) 5.93 5.92 29.05 89.93 90.13 120.04 pr: 294.47, r: 883.41 Peak table: 500(sub) 3238(all) Best cell: 440 indexed, Niggli cF( 1,12): 8.37 8.39 8.38 89.94 89.93 90.12 prim: 147.16, red: 588.62 Make subset: 0.00017 Make T-vectors: 0.40487 Make unit cell: 0.54145 UM TTT INFO: Volume check Primitive unit cell refinement volume check UB fit with 3031 obs out of 3238 (total:3244,skipped:6) (93.61%) UB - matrix: 0.038677 0.158531 0.069742 ( 0.000025 0.000030 0.000024 ) 0.134238 0.058145 0.068635 ( 0.000025 0.000030 0.000024 ) 0.043960 0.007267 -0.108992 ( 0.000021 0.000025 0.000020 ) M - matrix: 0.021448 0.014256 0.007120 ( 0.000007 0.000006 0.000005 ) 0.014256 0.028566 0.014255 ( 0.000006 0.000010 0.000006 ) 0.007120 0.014255 0.021454 ( 0.000005 0.000006 0.000006 ) unit cell: 5.9246(13) 5.9233(13) 5.9231(11) 119.92(2) 90.021(16) 119.93(2) V = 147.27(5) UB fit with 3028 obs out of 3238 (total:3244,skipped:6) (93.51%) UB - matrix: 0.038677 0.158523 0.069735 ( 0.000025 0.000030 0.000024 ) 0.134233 0.058158 0.068642 ( 0.000025 0.000030 0.000024 ) 0.043961 0.007274 -0.108989 ( 0.000021 0.000025 0.000020 ) M - matrix: 0.021447 0.014258 0.007120 ( 0.000007 0.000006 0.000005 ) 0.014258 0.028565 0.014254 ( 0.000006 0.000010 0.000006 ) 0.007120 0.014254 0.021453 ( 0.000005 0.000006 0.000006 ) unit cell: 5.9251(13) 5.9235(13) 5.9230(11) 119.92(2) 90.021(16) 119.94(2) V = 147.28(5) UB fit with 3028 obs out of 3238 (total:3244,skipped:6) (93.51%) UB - matrix: 0.038676 0.158523 0.069735 ( 0.000025 0.000030 0.000024 ) 0.134233 0.058158 0.068642 ( 0.000025 0.000030 0.000024 ) 0.043961 0.007274 -0.108989 ( 0.000021 0.000025 0.000020 ) M - matrix: 0.021447 0.014258 0.007120 ( 0.000007 0.000006 0.000005 ) 0.014258 0.028565 0.014254 ( 0.000006 0.000010 0.000006 ) 0.007120 0.014254 0.021453 ( 0.000005 0.000006 0.000006 ) unit cell: 5.9251(13) 5.9236(13) 5.9230(11) 119.92(2) 90.021(16) 119.94(2) V = 147.28(5) UM TTT INFO: Primitive unit cell refinement unsuccessful Primitive unit cell refinement UB fit with 3031 obs out of 3238 (total:3244,skipped:6) (93.61%) UB - matrix: 0.038677 0.158531 0.069742 ( 0.000025 0.000030 0.000024 ) 0.134238 0.058145 0.068635 ( 0.000025 0.000030 0.000024 ) 0.043960 0.007267 -0.108992 ( 0.000021 0.000025 0.000020 ) M - matrix: 0.021448 0.014256 0.007120 ( 0.000007 0.000006 0.000005 ) 0.014256 0.028566 0.014255 ( 0.000006 0.000010 0.000006 ) 0.007120 0.014255 0.021454 ( 0.000005 0.000006 0.000006 ) unit cell: 5.9246(13) 5.9233(13) 5.9231(11) 119.92(2) 90.021(16) 119.93(2) V = 147.27(5) No constraint UB - matrix: -0.025022 -0.079257 -0.015543 ( 0.000011 0.000012 0.000011 ) 0.072353 -0.029075 0.032807 ( 0.000011 0.000012 0.000011 ) -0.036175 -0.003635 0.076478 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007170 0.000011 -0.000004 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007140 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000004 -0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025022 -0.079257 -0.015543 ( 0.000011 0.000012 0.000011 ) 0.072353 -0.029075 0.032807 ( 0.000011 0.000012 0.000011 ) -0.036175 -0.003635 0.076478 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007156 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007156 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007156 ( 0.000000 0.000000 0.000001 ) UB fit with 2862 obs out of 3238 (total:3244,skipped:6) (88.39%) unit cell: 8.3769(11) 8.3941(11) 8.3785(10) 90.000(10) 89.968(10) 90.088(11) V = 589.14(13) unit cell: 8.3831(3) 8.3831(3) 8.3831(3) 90.0 90.0 90.0 V = 589.14(4) AUTO INFO: Dirax ended... Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" ******************************************************************************************************* Auto analyse stage: MODEL REFINEMENT (Tue Mar 27 15:39:25 2018) ******************************************************************************************************* UB fit with 2867 obs out of 3244 (total:3244,skipped:0) (88.38%) UB - matrix: -0.025019 -0.079257 -0.015544 ( 0.000011 0.000012 0.000011 ) 0.072352 -0.029077 0.032808 ( 0.000011 0.000012 0.000012 ) -0.036178 -0.003638 0.076480 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007170 0.000011 -0.000004 ( 0.000002 0.000001 0.000001 ) 0.000011 0.007140 -0.000000 ( 0.000001 0.000002 0.000001 ) -0.000004 -0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3769(11) 8.3940(11) 8.3783(10) 89.999(10) 89.965(10) 90.086(11) V = 589.13(13) OTKP changes: 214 2 4 6 Cycle 1 - Res: 0.022524, da=0.019053, sx=0.002880, sy=0.003774, h=0.005692, k=0.007184, l=0.006143, LM=0.000000 Cycle 2 - Res: 0.021880, da=0.018907, sx=0.002664, sy=0.003194, h=0.004949, k=0.006741, l=0.005833, LM=0.000000 Cycle 3 - Res: 0.021881, da=0.018908, sx=0.002664, sy=0.003193, h=0.004950, k=0.006742, l=0.005833, LM=0.000000 Cycle 4 - Res: 0.021881, da=0.018908, sx=0.002664, sy=0.003193, h=0.004950, k=0.006742, l=0.005833, LM=0.000000 Model change (all parameters): Omega Offset 0.002850 0.019729 0.0168793 7.3836e-007 1 Kappa Offset -0.132400 -0.132400 0 0 0 Phi Offset 0.000000 0.000000 0 0 0 Alpha Value 50.021780 50.021780 0 0 0 Beta Value -0.006110 -0.006110 0 0 0 Theta Offset -0.148000 -0.166580 -0.0185803 1.75288e-006 1 Det. D. Scale 53.000000 52.838453 -0.161547 1.05414e-006 1 Det. Offset X 1028.284000 1027.230739 -1.05326 3.85956e-005 1 Det. Offset Y 1027.509000 1025.273524 -2.23548 3.96836e-005 1 Det. Rot. X 0.746000 0.717416 -0.028584 7.71934e-007 1 Det. Rot. Y -0.076000 -0.123260 -0.0472604 1.65493e-006 1 Det. Rot. Z 0.000000 0.000000 0 0 0 Det. Pixel D 1.000000 1.000000 0 0 0 Det. Pixel X 1.000000 1.000000 0 0 0 Det. Pixel Y 1.000000 1.000000 0 0 0 Det. Alpha 90.000000 90.000000 0 0 0 Det. Beta 90.000000 90.000000 0 0 0 Det. Gamma 90.000000 90.000000 0 0 0 Beam. Rot. Y -0.009840 -0.037601 -0.0277612 8.49373e-007 1 Beam. Rot. Z 0.000000 0.000000 0 0 0 Cryst. Rot. X 2.688404 2.688055 -0.000348587 8.17785e-007 1 Cryst. Rot. Y -25.294453 -25.298103 -0.0036495 6.45035e-007 1 Cryst. Rot. Z -109.074857 -109.040392 0.0344643 9.76035e-007 1 Rec. latt. a* 0.119376 0.119439 6.32243e-005 1.52477e-009 1 Rec. latt. b* 0.119132 0.119384 0.000251259 1.76598e-009 1 Rec. latt. c* 0.119356 0.119390 3.42072e-005 1.76411e-009 1 Rec. latt. al* 90.001470 89.978164 -0.0233064 1.00064e-006 1 Rec. latt. be* 90.034662 89.967254 -0.0674088 9.76238e-007 1 Rec. latt. ga* 89.913937 89.961071 0.0471332 9.84989e-007 1 Cryst. Dance X 0.000000 0.000000 0 0 0 Cryst. Dance Y 0.000000 0.000000 0 0 0 Cryst. Dance Z 0.000000 0.000000 0 0 0 No constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072429 -0.029138 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036212 -0.003622 0.076457 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000004 0.000004 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007170 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000004 0.000003 0.007172 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072429 -0.029138 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036212 -0.003622 0.076457 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 2872 obs out of 3244 (total:3244,skipped:0) (88.53%) unit cell: 8.3704(10) 8.3769(11) 8.3756(10) 90.021(10) 90.033(9) 90.029(10) V = 587.28(12) unit cell: 8.3743(3) 8.3743(3) 8.3743(3) 90.0 90.0 90.0 V = 587.28(4) No constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072430 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000004 0.000004 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007170 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000004 0.000003 0.007172 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072430 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 2872 obs out of 3244 (total:3244,skipped:0) (88.53%) unit cell: 8.3703(10) 8.3769(11) 8.3755(10) 90.021(10) 90.032(9) 90.030(10) V = 587.27(12) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) No constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000004 0.000004 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007170 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000004 0.000003 0.007172 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 2872 obs out of 3244 (total:3244,skipped:0) (88.53%) unit cell: 8.3703(10) 8.3769(11) 8.3755(10) 90.021(10) 90.032(9) 90.030(10) V = 587.27(12) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) ******************************************************************************************************* Auto analyse stage: BRAVAIS LATTICE FINDING (Tue Mar 27 15:39:25 2018) ******************************************************************************************************* Bravais lattice type: F Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" 7068 peak locations are merged to 3244 profiles (Parameters: ofix = 2.00, otan(th) = 0.00) We have put 3244 unindexed peaks to the CrysAlis peak table (3244 with profile info) No constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000004 0.000004 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007170 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000004 0.000003 0.007172 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 2872 obs out of 3244 (total:3244,skipped:0) (88.53%) unit cell: 8.3702(10) 8.3769(11) 8.3755(10) 90.021(10) 90.032(9) 90.030(10) V = 587.27(12) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) -------------------EXPERIMENT TAB SUMMARY------------------- CELL Niggli 1 cubic F 88.388 %(2862/3244) 8.3769(11) 8.3941(11) 8.3785(10) 90.000(10) 89.968(10) 90.088(11) V = 589.14(13) ------------------------------------------------------------ AUTO INFO: Finished at Tue Mar 27 15:39:25 2018 DC PROFFIT INFO: Meta algorithm started DELETE INFO: Deleting rpi files... (D:\Data\xs1714a\tmp\xs1714a_proffitpea*.rpi) DELETE INFO: Deleting tab files... (D:\Data\xs1714a\tmp\xs1714a_proffitpea*.tab) DELETE INFO: Deleting tabbin files... (D:\Data\xs1714a\tmp\xs1714a_proffitpea*.tabbin) DELETE INFO: Deleting rrpprof files... (D:\Data\xs1714a\tmp\xs1714a*.rrpprof) DELETE INFO: Deleting rrpprofinfo files... (D:\Data\xs1714a\tmp\xs1714a*.rrpprofinfo) DELETE INFO: Deleting bbm files... (D:\Data\xs1714a\tmp\xs1714a*.bbm) DELETE INFO: Deleting pcorr files... (D:\Data\xs1714a\tmp\xs1714a*.pcorr) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\tmp\xs1714a*.dat) DELETE INFO: Deleting ppc2 files... (D:\Data\xs1714a\tmp\xs1714a*.ppc2) DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:39:27 2018) ID: 2932; threads 39; handles 878; mem 518744.00 (1237704.00)kB; time: 1w 5d 0h 44m 57s MEMORY INFO: Memory PF:0.0, Ph:229.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:2.0, Ph:229.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.4,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:39:27 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) 8.37024 ( 0.00097 ) 8.37691 ( 0.00106 ) 8.37554 ( 0.00098 ) 90.02113 ( 0.00986 ) 90.03240 ( 0.00940 ) 90.03043 ( 0.00981 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:39:27 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000010 0.000011 0.000011 ) 0.072431 -0.029136 0.032908 ( 0.000009 0.000010 0.000010 ) -0.036213 -0.003622 0.076458 ( 0.000009 0.000010 0.000010 ) M - matrix: 0.007181 0.000004 0.000004 ( 0.000002 0.000001 0.000001 ) 0.000004 0.007170 0.000003 ( 0.000001 0.000002 0.000001 ) 0.000004 0.000003 0.007172 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3702(10) 8.3769(11) 8.3755(10) 90.021(10) 90.032(9) 90.030(10) V = 587.27(12) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb PROFFITPEAK info: 312 peaks in the peak location table UB fit with 134 obs out of 150 (total:150,skipped:0) (89.33%) UB - matrix: -0.025030 -0.079635 -0.015605 ( 0.000091 0.000114 0.000050 ) 0.072749 -0.029674 0.032968 ( 0.000130 0.000162 0.000071 ) -0.035981 -0.003597 0.076553 ( 0.000051 0.000064 0.000028 ) M - matrix: 0.007214 -0.000036 0.000034 ( 0.000020 0.000015 0.000008 ) -0.000036 0.007235 -0.000011 ( 0.000015 0.000021 0.000009 ) 0.000034 -0.000011 0.007191 ( 0.000008 0.000009 0.000007 ) unit cell: 8.352(11) 8.339(11) 8.365(5) 89.91(7) 90.27(7) 89.71(11) V = 583(1) UB fit with 134 obs out of 150 (total:150,skipped:0) (89.33%) UB - matrix: -0.025030 -0.079635 -0.015605 ( 0.000091 0.000114 0.000050 ) 0.072749 -0.029674 0.032968 ( 0.000130 0.000162 0.000071 ) -0.035981 -0.003597 0.076553 ( 0.000051 0.000064 0.000028 ) M - matrix: 0.007214 -0.000036 0.000034 ( 0.000020 0.000015 0.000008 ) -0.000036 0.007235 -0.000011 ( 0.000015 0.000021 0.000009 ) 0.000034 -0.000011 0.007191 ( 0.000008 0.000009 0.000007 ) unit cell: 8.352(11) 8.339(11) 8.365(5) 89.91(7) 90.27(7) 89.71(11) V = 583(1) OTKP changes: 25 1 1 1 No constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007172 -0.000032 0.000032 ( 0.000019 0.000015 0.000008 ) -0.000032 0.007180 0.000006 ( 0.000015 0.000021 0.000008 ) 0.000032 0.000006 0.007146 ( 0.000008 0.000008 0.000006 ) Constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007128 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.007128 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.007128 ( 0.000000 0.000000 0.000003 ) UB fit with 136 obs out of 150 (total:150,skipped:0) (90.67%) unit cell: 8.376(11) 8.371(12) 8.391(5) 90.05(7) 90.26(7) 89.74(11) V = 588(1) unit cell: 8.3792(15) 8.3792(15) 8.3792(15) 90.0 90.0 90.0 V = 588.31(18) UB fit with 136 obs out of 150 (total:150,skipped:0) (90.67%) UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007172 -0.000032 0.000032 ( 0.000019 0.000015 0.000008 ) -0.000032 0.007180 0.000006 ( 0.000015 0.000021 0.000008 ) 0.000032 0.000006 0.007146 ( 0.000008 0.000008 0.000006 ) unit cell: 8.376(11) 8.371(12) 8.391(5) 90.05(7) 90.26(7) 89.74(11) V = 588(1) OTKP changes: 25 1 1 1 No constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007172 -0.000032 0.000032 ( 0.000019 0.000015 0.000008 ) -0.000032 0.007180 0.000006 ( 0.000015 0.000021 0.000008 ) 0.000032 0.000006 0.007146 ( 0.000008 0.000008 0.000006 ) Constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007128 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.007128 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.007128 ( 0.000000 0.000000 0.000003 ) UB fit with 136 obs out of 150 (total:150,skipped:0) (90.67%) unit cell: 8.376(11) 8.371(12) 8.391(5) 90.05(7) 90.26(7) 89.74(11) V = 588(1) unit cell: 8.3792(15) 8.3792(15) 8.3792(15) 90.0 90.0 90.0 V = 588.31(18) 150 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.093) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007172 -0.000032 0.000032 ( 0.000019 0.000015 0.000008 ) -0.000032 0.007180 0.000006 ( 0.000015 0.000021 0.000008 ) 0.000032 0.000006 0.007146 ( 0.000008 0.000008 0.000006 ) Constraint UB - matrix: -0.025146 -0.079309 -0.015606 ( 0.000095 0.000119 0.000051 ) 0.072415 -0.029648 0.032935 ( 0.000126 0.000157 0.000068 ) -0.035992 -0.003349 0.076271 ( 0.000046 0.000058 0.000025 ) M - matrix: 0.007128 0.000000 0.000000 ( 0.000003 0.000000 0.000000 ) 0.000000 0.007128 0.000000 ( 0.000000 0.000003 0.000000 ) 0.000000 0.000000 0.007128 ( 0.000000 0.000000 0.000003 ) UB fit with 136 obs out of 150 (total:150,skipped:0) (90.67%) unit cell: 8.376(11) 8.371(12) 8.391(5) 90.05(7) 90.26(7) 89.74(11) V = 588(1) unit cell: 8.3792(15) 8.3792(15) 8.3792(15) 90.0 90.0 90.0 V = 588.31(18) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 135 obs out of 150 (total:150,skipped:0) (90.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb 2 of 117 peaks identified as outliers and rejected 115 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 115 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 115 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.15- 1.70 | 12 | 0.918 ( 0.153) | 1.255 ( 0.651) | 1.123 ( 0.546) | 1.61- 1.27 | 12 | 0.971 ( 0.104) | 1.094 ( 0.251) | 1.012 ( 0.449) | 1.26- 1.09 | 12 | 1.013 ( 0.061) | 1.049 ( 0.087) | 1.294 ( 0.579) | 1.09- 0.92 | 12 | 0.977 ( 0.079) | 1.050 ( 0.067) | 0.862 ( 0.260) | 0.92- 0.84 | 12 | 1.019 ( 0.084) | 1.056 ( 0.148) | 1.156 ( 0.385) | 0.84- 0.76 | 12 | 0.984 ( 0.074) | 0.959 ( 0.114) | 1.096 ( 0.453) | 0.76- 0.72 | 12 | 0.961 ( 0.062) | 0.871 ( 0.080) | 1.270 ( 0.565) | 0.72- 0.67 | 12 | 0.957 ( 0.055) | 0.864 ( 0.050) | 1.347 ( 0.451) | 0.67- 0.62 | 12 | 0.935 ( 0.038) | 0.822 ( 0.036) | 1.339 ( 0.506) | 0.62- 0.59 | 7 | 0.928 ( 0.059) | 0.801 ( 0.030) | 1.535 ( 0.479) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.15- 0.59 | 115 | 0.968 ( 0.090) | 0.990 ( 0.273) | 1.189 ( 0.506) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) UB - matrix: -0.025200 -0.079410 -0.015390 ( 0.000063 0.000074 0.000032 ) 0.072233 -0.029273 0.032859 ( 0.000064 0.000075 0.000032 ) -0.036061 -0.003361 0.076341 ( 0.000038 0.000045 0.000020 ) M - matrix: 0.007153 0.000008 0.000008 ( 0.000010 0.000008 0.000005 ) 0.000008 0.007174 0.000004 ( 0.000008 0.000013 0.000005 ) 0.000008 0.000004 0.007145 ( 0.000005 0.000005 0.000004 ) unit cell: 8.387(5) 8.374(7) 8.392(3) 90.03(4) 90.07(4) 90.06(6) V = 589.3(7) OTKP changes: 115 1 1 1 No constraint UB - matrix: -0.025241 -0.079296 -0.015646 ( 0.000050 0.000058 0.000025 ) 0.072342 -0.029497 0.032900 ( 0.000062 0.000072 0.000031 ) -0.036071 -0.003490 0.076518 ( 0.000035 0.000041 0.000018 ) M - matrix: 0.007172 -0.000007 0.000015 ( 0.000010 0.000007 0.000004 ) -0.000007 0.007170 0.000003 ( 0.000007 0.000010 0.000005 ) 0.000015 0.000003 0.007182 ( 0.000004 0.000005 0.000004 ) Constraint UB - matrix: -0.025241 -0.079296 -0.015646 ( 0.000050 0.000058 0.000025 ) 0.072342 -0.029497 0.032900 ( 0.000062 0.000072 0.000031 ) -0.036071 -0.003490 0.076518 ( 0.000035 0.000041 0.000018 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 8.376(5) 8.377(6) 8.370(3) 90.03(4) 90.12(4) 89.95(5) V = 587.2(6) unit cell: 8.3740(8) 8.3740(8) 8.3740(8) 90.0 90.0 90.0 V = 587.21(10) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.950) HKL list info: 270 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025241 -0.079296 -0.015646 ( 0.000050 0.000058 0.000025 ) 0.072342 -0.029497 0.032900 ( 0.000062 0.000072 0.000031 ) -0.036071 -0.003490 0.076518 ( 0.000035 0.000041 0.000018 ) M - matrix: 0.007172 -0.000007 0.000015 ( 0.000010 0.000007 0.000004 ) -0.000007 0.007170 0.000003 ( 0.000007 0.000010 0.000005 ) 0.000015 0.000003 0.007182 ( 0.000004 0.000005 0.000004 ) Constraint UB - matrix: -0.025241 -0.079296 -0.015646 ( 0.000050 0.000058 0.000025 ) 0.072342 -0.029497 0.032900 ( 0.000062 0.000072 0.000031 ) -0.036071 -0.003490 0.076518 ( 0.000035 0.000041 0.000018 ) M - matrix: 0.007162 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007162 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007162 ( 0.000000 0.000000 0.000001 ) UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) unit cell: 8.376(5) 8.377(6) 8.370(3) 90.03(4) 90.12(4) 89.95(5) V = 587.2(6) unit cell: 8.3740(8) 8.3740(8) 8.3740(8) 90.0 90.0 90.0 V = 587.21(10) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 115 obs out of 115 (total:115,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb 2 of 115 peaks identified as outliers and rejected 113 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 113 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 113 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 1.61 | 11 | 0.947 ( 0.121) | 1.016 ( 0.174) | 1.048 ( 0.560) | 1.61- 1.28 | 11 | 0.988 ( 0.099) | 1.190 ( 0.365) | 1.012 ( 0.477) | 1.26- 1.09 | 11 | 1.015 ( 0.062) | 1.079 ( 0.115) | 1.243 ( 0.609) | 1.09- 0.96 | 11 | 0.991 ( 0.072) | 1.068 ( 0.070) | 0.887 ( 0.413) | 0.96- 0.88 | 11 | 0.993 ( 0.091) | 1.005 ( 0.150) | 1.168 ( 0.492) | 0.85- 0.82 | 11 | 0.996 ( 0.081) | 0.994 ( 0.129) | 0.963 ( 0.213) | 0.81- 0.73 | 11 | 0.983 ( 0.053) | 0.911 ( 0.080) | 1.380 ( 0.560) | 0.73- 0.69 | 11 | 0.971 ( 0.054) | 0.861 ( 0.057) | 1.381 ( 0.587) | 0.69- 0.64 | 11 | 0.943 ( 0.047) | 0.837 ( 0.048) | 1.164 ( 0.335) | 0.64- 0.59 | 14 | 0.922 ( 0.051) | 0.811 ( 0.032) | 1.503 ( 0.500) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 0.59 | 113 | 0.974 ( 0.081) | 0.973 ( 0.191) | 1.184 ( 0.527) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.0 | 236 | 1.117 ( 0.131) | 1.236 ( 0.475) | 1.257 ( 1.131) | 13.1-18.9 | 236 | 1.078 ( 0.053) | 1.133 ( 0.273) | 1.177 ( 0.510) | 18.9-23.0 | 236 | 1.066 ( 0.068) | 1.134 ( 0.370) | 1.166 ( 0.535) | 23.0-27.1 | 236 | 1.032 ( 0.075) | 1.068 ( 0.248) | 1.155 ( 0.546) | 27.1-30.7 | 236 | 1.010 ( 0.071) | 1.002 ( 0.174) | 1.204 ( 0.500) | 30.7-33.8 | 236 | 0.979 ( 0.078) | 0.926 ( 0.096) | 1.199 ( 0.521) | 33.8-36.9 | 236 | 0.959 ( 0.074) | 0.906 ( 0.121) | 1.169 ( 0.476) | 37.0-39.7 | 236 | 0.942 ( 0.084) | 0.870 ( 0.130) | 1.229 ( 0.552) | 39.7-42.7 | 236 | 0.919 ( 0.075) | 0.836 ( 0.079) | 1.197 ( 0.549) | 42.7-49.9 | 240 | 0.925 ( 0.085) | 0.809 ( 0.063) | 1.152 ( 0.475) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2364 | 1.003 ( 0.105) | 0.992 ( 0.277) | 1.191 ( 0.609) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0019 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 23819788 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 15:39:56 2018 PROFFITMAIN - Started at Tue Mar 27 15:39:56 2018 OTKP changes: 2358 2 4 6 OTKP changes: 2358 2 4 6 No constraint UB - matrix: -0.025029 -0.079523 -0.015580 ( 0.000006 0.000007 0.000006 ) 0.072516 -0.029189 0.032937 ( 0.000005 0.000006 0.000006 ) -0.036233 -0.003601 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007198 0.000004 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007189 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000002 0.007187 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025029 -0.079523 -0.015580 ( 0.000006 0.000007 0.000006 ) 0.072516 -0.029189 0.032937 ( 0.000005 0.000006 0.000006 ) -0.036233 -0.003601 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) UB fit with 2361 obs out of 2364 (total:2364,skipped:0) (99.87%) unit cell: 8.3604(5) 8.3656(6) 8.3665(5) 90.015(5) 90.038(5) 90.033(6) V = 585.15(7) unit cell: 8.36418(16) 8.36418(16) 8.36418(16) 90.0 90.0 90.0 V = 585.154(19) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024859 -0.079568 -0.015653 ( 0.000013 0.000015 0.000011 ) 0.072454 -0.029195 0.032945 ( 0.000016 0.000018 0.000013 ) -0.036280 -0.003652 0.076382 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000005 0.000005 ( 0.000003 0.000002 0.000001 ) -0.000005 0.007197 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000005 0.000005 0.007165 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3686(15) 8.3611(15) 8.3798(10) 90.038(12) 90.039(12) 89.961(14) V = 586.34(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024989 -0.079526 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072497 -0.029265 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036260 -0.003621 0.076515 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000003 0.000005 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000010 0.007184 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3621(11) 8.3627(14) 8.3686(11) 89.923(12) 90.042(11) 89.976(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3576(14) 8.3628(11) 89.935(12) 90.003(11) 89.964(12) V = 584.02(15) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3576(14) 8.3628(11) 89.935(12) 90.003(11) 89.964(12) V = 584.02(15) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025024 -0.079572 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072542 -0.029297 0.032984 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003569 0.076592 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3576(14) 8.3628(11) 89.935(12) 90.003(11) 89.964(12) V = 584.02(15) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025025 -0.079531 -0.015717 ( 0.000008 0.000013 0.000012 ) 0.072407 -0.029344 0.032917 ( 0.000008 0.000014 0.000014 ) -0.036197 -0.003662 0.076525 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007179 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000004 0.007187 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3712(11) 8.3594(12) 8.3670(11) 90.031(11) 90.054(11) 89.985(11) V = 585.51(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3667(10) 8.3560(12) 8.3597(11) 89.995(11) 90.023(10) 90.025(11) V = 584.44(13) unit cell: 8.3608(3) 8.3608(3) 8.3608(3) 90.0 90.0 90.0 V = 584.44(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3667(10) 8.3560(12) 8.3597(11) 89.995(11) 90.023(10) 90.025(11) V = 584.44(13) unit cell: 8.3608(3) 8.3608(3) 8.3608(3) 90.0 90.0 90.0 V = 584.44(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079555 -0.015727 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032981 ( 0.000008 0.000014 0.000013 ) -0.036292 -0.003696 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3667(10) 8.3560(12) 8.3597(11) 89.995(11) 90.023(10) 90.025(11) V = 584.44(13) unit cell: 8.3608(3) 8.3608(3) 8.3608(3) 90.0 90.0 90.0 V = 584.44(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025243 -0.079444 -0.015763 ( 0.000011 0.000016 0.000017 ) 0.072357 -0.029416 0.032793 ( 0.000008 0.000011 0.000012 ) -0.036252 -0.003617 0.076601 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007187 0.000008 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007190 0.000011 ( 0.000001 0.000003 0.000002 ) -0.000006 0.000011 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3668(10) 8.3652(14) 8.3641(11) 90.085(12) 89.950(10) 90.064(12) V = 585.40(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3603(10) 8.3611(14) 8.3567(11) 90.050(12) 89.990(10) 90.063(11) V = 584.15(14) unit cell: 8.3594(3) 8.3594(3) 8.3594(3) 90.0 90.0 90.0 V = 584.15(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3603(10) 8.3611(14) 8.3567(11) 90.050(12) 89.990(10) 90.063(11) V = 584.15(14) unit cell: 8.3594(3) 8.3594(3) 8.3594(3) 90.0 90.0 90.0 V = 584.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079485 -0.015743 ( 0.000011 0.000015 0.000017 ) 0.072457 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036198 -0.003652 0.076683 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3603(10) 8.3611(14) 8.3567(11) 90.050(12) 89.990(10) 90.063(11) V = 584.15(14) unit cell: 8.3594(3) 8.3594(3) 8.3594(3) 90.0 90.0 90.0 V = 584.15(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 113 obs out of 113 (total:113,skipped:0) (100.00%) UB - matrix: -0.025203 -0.079408 -0.015588 ( 0.000058 0.000068 0.000029 ) 0.072363 -0.029440 0.032867 ( 0.000062 0.000072 0.000031 ) -0.036070 -0.003612 0.076564 ( 0.000037 0.000043 0.000019 ) M - matrix: 0.007173 0.000001 0.000010 ( 0.000010 0.000008 0.000004 ) 0.000001 0.007185 -0.000006 ( 0.000008 0.000012 0.000005 ) 0.000010 -0.000006 0.007185 ( 0.000004 0.000005 0.000004 ) unit cell: 8.375(5) 8.368(6) 8.368(3) 89.95(4) 90.08(4) 90.01(6) V = 586.4(6) OTKP changes: 113 1 1 1 No constraint UB - matrix: -0.025283 -0.079330 -0.015682 ( 0.000055 0.000065 0.000028 ) 0.072376 -0.029483 0.032876 ( 0.000062 0.000072 0.000031 ) -0.036078 -0.003502 0.076543 ( 0.000032 0.000037 0.000016 ) M - matrix: 0.007179 -0.000002 0.000014 ( 0.000010 0.000007 0.000004 ) -0.000002 0.007175 0.000007 ( 0.000007 0.000011 0.000005 ) 0.000014 0.000007 0.007186 ( 0.000004 0.000005 0.000003 ) Constraint UB - matrix: -0.025283 -0.079330 -0.015682 ( 0.000055 0.000065 0.000028 ) 0.072376 -0.029483 0.032876 ( 0.000062 0.000072 0.000031 ) -0.036078 -0.003502 0.076543 ( 0.000032 0.000037 0.000016 ) M - matrix: 0.007170 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007170 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007170 ( 0.000000 0.000000 0.000001 ) UB fit with 113 obs out of 113 (total:113,skipped:0) (100.00%) unit cell: 8.371(5) 8.374(6) 8.368(3) 90.05(4) 90.11(4) 89.99(6) V = 586.6(6) unit cell: 8.3709(9) 8.3709(9) 8.3709(9) 90.0 90.0 90.0 V = 586.57(11) Run 6 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.904) HKL list info: 265 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025283 -0.079330 -0.015682 ( 0.000055 0.000065 0.000028 ) 0.072376 -0.029483 0.032876 ( 0.000062 0.000072 0.000031 ) -0.036078 -0.003502 0.076543 ( 0.000032 0.000037 0.000016 ) M - matrix: 0.007179 -0.000002 0.000014 ( 0.000010 0.000007 0.000004 ) -0.000002 0.007175 0.000007 ( 0.000007 0.000011 0.000005 ) 0.000014 0.000007 0.007186 ( 0.000004 0.000005 0.000003 ) Constraint UB - matrix: -0.025283 -0.079330 -0.015682 ( 0.000055 0.000065 0.000028 ) 0.072376 -0.029483 0.032876 ( 0.000062 0.000072 0.000031 ) -0.036078 -0.003502 0.076543 ( 0.000032 0.000037 0.000016 ) M - matrix: 0.007170 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007170 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007170 ( 0.000000 0.000000 0.000001 ) UB fit with 113 obs out of 113 (total:113,skipped:0) (100.00%) unit cell: 8.371(5) 8.374(6) 8.368(3) 90.05(4) 90.11(4) 89.99(6) V = 586.6(6) unit cell: 8.3709(9) 8.3709(9) 8.3709(9) 90.0 90.0 90.0 V = 586.57(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 113 obs out of 113 (total:113,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: 0.084729 -0.000009 0.000165 ( 0.000055 0.000064 0.000028 ) -0.000008 0.084698 0.000092 ( 0.000062 0.000072 0.000031 ) 0.000005 -0.000007 0.084766 ( 0.000032 0.000038 0.000016 ) M - matrix: 0.007179 -0.000001 0.000014 ( 0.000009 0.000008 0.000004 ) -0.000001 0.007174 0.000007 ( 0.000008 0.000012 0.000004 ) 0.000014 0.000007 0.007185 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: 0.084729 -0.000009 0.000165 ( 0.000055 0.000064 0.000028 ) -0.000008 0.084698 0.000092 ( 0.000062 0.000072 0.000031 ) 0.000005 -0.000007 0.084766 ( 0.000032 0.000038 0.000016 ) M - matrix: 0.007169 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007169 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007169 ( 0.000000 0.000000 0.000001 ) UB fit with 113 obs out of 113 (total:113,skipped:0) (100.00%) unit cell: 8.371(5) 8.374(7) 8.3678(16) 90.06(3) 90.11(3) 89.99(6) V = 586.6(6) unit cell: 8.3712(9) 8.3712(9) 8.3712(9) 90.0 90.0 90.0 V = 586.63(11) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025012 -0.079448 -0.015553 ( 0.000006 0.000007 0.000007 ) 0.072506 -0.029147 0.032897 ( 0.000006 0.000007 0.000007 ) -0.036223 -0.003578 0.076522 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 0.000003 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007174 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025012 -0.079448 -0.015553 ( 0.000006 0.000007 0.000007 ) 0.072506 -0.029147 0.032897 ( 0.000006 0.000007 0.000007 ) -0.036223 -0.003578 0.076522 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 2361 obs out of 2364 (total:2364,skipped:0) (99.87%) unit cell: 8.3622(6) 8.3741(7) 8.3709(5) 90.024(6) 90.019(5) 90.027(6) V = 586.18(7) unit cell: 8.3691(2) 8.3691(2) 8.3691(2) 90.0 90.0 90.0 V = 586.18(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 69 reflections under beam stop or inside a detector rejection region 21 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3194 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:40:02 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) Run 6 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.904) PROFFIT INFO: signal sum: min=255.0000 max=20874476.0000 PROFFIT INFO: signal sum lp corr: min=469.0837 max=2959127.5275 PROFFIT INFO: background sum: min=619.0000 max=27145.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=12660.0000 PROFFIT INFO: num of signal pixels: min=51 max=581 PROFFIT INFO: Inet: min=750.5339 max=4734604.0000 PROFFIT INFO: sig(Inet): min=120.2540 max=47814.4414 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.84 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 34 155 333 646 728 1306 2131 2928 3194 Percent 0.0 0.0 1.1 4.9 10.4 20.2 22.8 40.9 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3194 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3194 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4734604- 1119279 319 1848630.01 122.31 100.00 1118986- 626139 319 849822.25 102.56 100.00 626072- 264851 319 414753.15 94.95 100.00 264400- 169691 319 203033.23 71.57 100.00 169588- 120511 319 144763.19 51.07 100.00 120504- 93887 319 105917.16 36.26 100.00 93768- 66277 319 80968.27 29.39 100.00 66195- 5636 319 37671.53 19.29 100.00 5631- 2961 319 3962.09 5.31 96.87 2959- 751 323 2128.25 3.78 55.11 ------------------------------------------------------------------------------------ 4734604- 751 3194 368705.26 53.59 95.15 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 733368.40 93.81 100.00 1.41- 1.12 319 599058.12 63.24 99.37 1.12- 0.96 319 502703.49 71.10 97.81 0.96- 0.88 319 351975.13 59.90 94.67 0.88- 0.81 319 450922.32 68.79 99.69 0.81- 0.73 319 248711.35 41.61 94.98 0.73- 0.71 319 176343.23 34.23 88.40 0.71- 0.65 319 318721.44 48.09 94.04 0.65- 0.62 319 154899.52 27.55 87.77 0.62- 0.58 323 153053.65 27.87 94.74 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 368705.26 53.59 95.15 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:40:03 2018 Sorting 3194 observations 119 unique observations with > 7.00 F2/sig(F2) 3194 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 24 546 Total number of frames 546 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3194 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 4 111 Total number of frames 111 2569 observations > 7.00 F2/sig(F2) 2569 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 4 111 Total number of frames 111 Removing 'redundancy=1' reflections Average redundancy: 20.3 (Out of 2569 removed 7 = 2562, unique = 126) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2562 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 4 111 Total number of frames 111 126 unique data precomputed (should be 126) 126 unique data with 2562 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.3 (Out of 2562 removed 0 = 2562, unique = 126) 126 unique data precomputed (should be 126) 126 unique data with 2562 observations RMS deviation of equivalent data = 0.25959 Rint = 0.18969 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18209, wR= 0.26980 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13618, wR= 0.17539, Acormin=0.600, Acormax=1.407, Acor_av=0.981 F test: Probability=1.000, F= 1.784 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11827, wR= 0.15017, Acormin=0.565, Acormax=1.450, Acor_av=0.913 F test: Probability=1.000, F= 1.324 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10630, wR= 0.14207, Acormin=0.591, Acormax=1.549, Acor_av=0.948 F test: Probability=1.000, F= 1.235 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09085, wR= 0.12062, Acormin=0.518, Acormax=1.573, Acor_av=0.883 F test: Probability=1.000, F= 1.367 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07799, wR= 0.10942, Acormin=0.496, Acormax=1.612, Acor_av=0.898 F test: Probability=1.000, F= 1.353 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09889, wR= 0.13565, Acormin=0.606, Acormax=1.616, Acor_av=0.957 F test: Probability=0.000, F= 0.621 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08460, wR= 0.11551, Acormin=0.497, Acormax=1.606, Acor_av=0.890 F test: Probability=0.000, F= 0.848 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07524, wR= 0.10573, Acormin=0.485, Acormax=1.642, Acor_av=0.905 F test: Probability=0.947, F= 1.068 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07415, wR= 0.10284, Acormin=0.364, Acormax=1.459, Acor_av=0.803 F test: Probability=0.987, F= 1.095 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09924, wR= 0.13051, Acormin=0.444, Acormax=1.469, Acor_av=0.835 F test: Probability=0.000, F= 0.559 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08262, wR= 0.11086, Acormin=0.483, Acormax=1.603, Acor_av=0.882 F test: Probability=0.000, F= 0.806 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08299, wR= 0.11049, Acormin=0.109, Acormax=0.400, Acor_av=0.218 F test: Probability=0.000, F= 0.796 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07249, wR= 0.09965, Acormin=0.115, Acormax=0.450, Acor_av=0.249 F test: Probability=0.823, F= 1.039 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06543, wR= 0.09093, Acormin=0.136, Acormax=0.506, Acor_av=0.263 F test: Probability=1.000, F= 1.267 Final absorption model (ne=6, no=5): Rint= 0.07415, Acormin=0.364, Acormax=1.459, Acor_av=0.803 Combined refinement in use Rint: 0.18978 There are 111 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 158 pars with 12561 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25959 Using Levenberg-Marquardt: 0.00010 New wR= 0.05921 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18969 with corrections 0.04654 Rint for all data: 0.18978 with corrections 0.04676 0 observations identified as outliers and rejected Cycle 2 wR= 0.05921 Using Levenberg-Marquardt: 0.00001 New wR= 0.05656 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18969 with corrections 0.04431 Rint for all data: 0.18978 with corrections 0.04453 0 observations identified as outliers and rejected Cycle 3 wR= 0.05656 Using Levenberg-Marquardt: 0.00000 New wR= 0.05599 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18969 with corrections 0.04386 Rint for all data: 0.18978 with corrections 0.04408 0 observations identified as outliers and rejected Cycle 4 wR= 0.05599 Using Levenberg-Marquardt: 0.00000 New wR= 0.05568 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18969 with corrections 0.04359 Rint for all data: 0.18978 with corrections 0.04381 0 observations identified as outliers and rejected Cycle 5 wR= 0.05568 Using Levenberg-Marquardt: 0.00000 New wR= 0.05549 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18969 with corrections 0.04343 Rint for all data: 0.18978 with corrections 0.04365 0 observations identified as outliers and rejected Final wR= 0.05549 Final frame scales: Min= 0.7166 Max= 1.2363 Final absorption correction factors: Amin= 0.4890 Amax= 1.3870 PROFFIT INFO: Inet (after scale3 abspack): min=780.1188 max=4534867.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=107.0198 max=53184.4766 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3194 reflections read from tmp file 636 reflections are rejected (635 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 5 2 4 3 6 3 11 117 Initial Chi^2= 0.41373 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.92313 Current error model SIG(F2)^2 = 153.21*I_RAW + 0.00*I_BACK+(0.01629*)^2 Cycle 2, Chi^2= 1.01103 Current error model SIG(F2)^2 = 105.29*I_RAW + 0.00*I_BACK+(0.02210*)^2 Cycle 3, Chi^2= 1.00053 Current error model SIG(F2)^2 = 113.82*I_RAW + 0.00*I_BACK+(0.02051*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 113.00*I_RAW + 0.00*I_BACK+(0.02070*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 113.13*I_RAW + 0.00*I_BACK+(0.02068*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 113.13*I_RAW + 0.00*I_BACK+(0.02068*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4534867- 1082162 319 1737870.43 45.03 100.00 1080073- 606990 319 808809.74 37.90 100.00 605912- 254380 319 402352.14 36.63 100.00 254281- 153757 319 191726.91 31.85 100.00 153743- 124504 319 138994.86 26.02 100.00 124034- 87448 319 102120.62 20.02 100.00 87405- 68356 319 78654.02 17.16 100.00 68330- 4933 319 39886.24 12.33 100.00 4931- 2730 319 3630.26 4.70 96.87 2729- 780 323 2145.57 3.89 78.02 ------------------------------------------------------------------------------------ 4534867- 780 3194 350182.67 23.53 97.46 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 732552.82 36.98 100.00 1.41- 1.12 319 580531.81 28.86 99.37 1.12- 0.96 319 458987.91 28.10 98.75 0.96- 0.88 319 330756.27 24.10 97.81 0.88- 0.81 319 424999.71 27.58 99.69 0.81- 0.73 319 228574.81 19.28 96.87 0.73- 0.71 319 165700.93 17.61 93.42 0.71- 0.65 319 297329.44 22.78 97.81 0.65- 0.62 319 144097.43 14.83 93.73 0.62- 0.58 323 140919.55 15.27 97.21 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 350182.67 23.53 97.46 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 732552.82 36.98 100.00 4.82- 1.12 638 656542.32 32.92 99.69 4.82- 0.96 957 590690.85 31.31 99.37 4.82- 0.88 1276 525707.20 29.51 98.98 4.82- 0.81 1595 505565.70 29.12 99.12 4.82- 0.73 1914 459400.56 27.48 98.75 4.82- 0.71 2233 417443.47 26.07 97.98 4.82- 0.65 2552 402429.21 25.66 97.96 4.82- 0.62 2871 373725.68 24.46 97.49 4.82- 0.58 3194 350182.67 23.53 97.46 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 350182.67 23.53 97.46 Scale applied to data: s=0.220513 (maximum obs:4534867.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.044; Rsigma 0.028: data 3194 -> merged 157 With outlier rejection... Rint 0.043; Rsigma 0.028: data 3177 -> merged 157 Rejected total: 17, method kkm 16, method Blessing 1 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585951, 4.831878 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 18.29 100.00 256 1.41 - 1.12 14 14 26.21 100.00 367 1.12 - 0.97 14 14 26.14 100.00 366 0.96 - 0.84 14 14 28.07 100.00 393 0.84 - 0.78 14 14 21.43 100.00 300 0.78 - 0.73 14 14 22.43 100.00 314 0.73 - 0.69 14 14 20.86 100.00 292 0.69 - 0.66 14 14 17.86 100.00 250 0.65 - 0.63 14 14 18.36 100.00 257 0.63 - 0.60 14 14 16.36 100.00 229 --------------------------------------------------------------- 8.37 - 0.60 140 140 21.60 100.00 3024 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:40:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362190 8.374076 8.370917 90.0242 90.0193 90.0272 3177 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1631 0 2131 2128 3177 N (int>3sigma) = 0 0 0 0 1631 0 2076 2069 3096 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 77.3 79.9 77.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 23.6 23.8 23.5 Lattice type: F chosen Volume: 586.18 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.97 90.06 119.93 Niggli form: a.a = 34.988 b.b = 34.996 c.c = 35.011 b.c = -17.487 a.c = -0.037 a.b = -17.460 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.084 CUBIC F-lattice R(int) = 0.043 [ 3020] Vol = 586.2 Cell: 8.362 8.374 8.371 89.98 89.98 90.03 Volume: 586.18 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.083 RHOMBOHEDRAL R-lattice R(int) = 0.048 [ 2741] Vol = 439.6 Cell: 5.916 5.915 14.498 89.97 90.05 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.083 RHOMBOHEDRAL R-lattice R(int) = 0.039 [ 873] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.498 89.97 90.05 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.061 TETRAGONAL I-lattice R(int) = 0.042 [ 2771] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.01 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.042 [ 2771] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.01 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.042 [ 2718] Vol = 293.1 Cell: 5.921 8.362 5.919 89.97 89.98 89.99 Volume: 293.09 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.041 [ 2368] Vol = 293.1 Cell: 8.362 5.921 5.919 90.02 90.03 89.99 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.050 MONOCLINIC I-lattice R(int) = 0.040 [ 2371] Vol = 293.1 Cell: 5.917 5.915 8.374 89.96 90.00 89.94 Volume: 293.09 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC C-lattice R(int) = 0.040 [ 2381] Vol = 293.1 Cell: 8.362 8.374 5.915 89.96 134.96 90.03 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.038 [ 1718] Vol = 146.5 Cell: 5.915 5.916 5.917 119.97 90.06 119.93 Volume: 146.54 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1631 0 2128 2131 3177 N (int>3sigma) = 0 0 0 0 1631 0 2069 2076 3096 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 79.9 77.3 77.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 23.8 23.6 23.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.173 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 232 714 N I>3s 32 32 221 714 0.9 0.9 0.7 36.8 8.5 8.5 5.3 27.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.043 2808 Fd-3m 1 1 227 C N N N N 37 2284 0.043 2847 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362190 8.374076 8.370917 89.9758 89.9807 90.0272 ZERR 3.00 0.000611 0.000705 0.000511 0.0059 0.0055 0.0064 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3879735- 744916 523 522 26 20.1 1405122.88 42.68 0.038 0.051 742862- 221705 495 492 26 18.9 443895.78 36.62 0.056 0.072 218848- 97100 742 742 26 28.5 147519.02 26.60 0.040 0.052 95247- 70085 511 508 26 19.5 82209.53 17.36 0.065 0.081 65263- 3606 416 411 26 15.8 26150.59 9.27 0.080 0.105 3363- 1703 507 502 27 18.6 2620.57 4.26 0.185 0.238 ------------------------------------------------------------------------------------------- 3879735- 1703 3194 3177 157 20.2 351009.08 23.54 0.043 0.058 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 595 587 26 22.6 600013.07 32.24 0.045 0.062 0.023 1.12-0.88 704 703 26 27.0 458285.88 27.38 0.032 0.041 0.025 0.85-0.75 594 594 26 22.8 325308.74 22.97 0.037 0.046 0.029 0.74-0.68 520 516 26 19.8 256152.07 20.62 0.050 0.059 0.033 0.67-0.63 488 487 26 18.7 149056.44 16.34 0.069 0.088 0.041 0.62-0.59 293 290 27 10.7 147499.48 15.15 0.072 0.078 0.041 ------------------------------------------------------------------------------------------------------ inf-0.59 3194 3177 157 20.2 351009.08 23.54 0.043 0.058 0.028 inf-0.60 3037 3022 139 21.7 363407.04 24.03 0.043 0.057 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 587 26 26 100.0 22.6 600013.07 167.08 0.045 0.006 1.12-0.88 703 26 26 100.0 27.0 458285.88 145.41 0.032 0.005 0.85-0.75 594 26 26 100.0 22.8 325308.74 116.58 0.037 0.006 0.74-0.68 516 26 26 100.0 19.8 256152.07 93.94 0.050 0.008 0.67-0.63 487 26 26 100.0 18.7 149056.44 70.11 0.069 0.010 0.62-0.59 290 27 27 100.0 10.7 147499.48 58.05 0.072 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3177 157 157 100.0 20.2 351009.08 116.15 0.043 0.007 inf-0.60 3022 139 139 100.0 21.7 363407.04 119.60 0.043 0.007 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025012 -0.079448 -0.015553 ( 0.000006 0.000007 0.000007 ) 0.072506 -0.029147 0.032897 ( 0.000006 0.000007 0.000007 ) -0.036223 -0.003578 0.076522 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 0.000003 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007174 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025012 -0.079448 -0.015553 ( 0.000006 0.000007 0.000007 ) 0.072506 -0.029147 0.032897 ( 0.000006 0.000007 0.000007 ) -0.036223 -0.003578 0.076522 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3622(6) 8.3741(7) 8.3709(5) 90.024(6) 90.019(5) 90.027(6) V = 586.18(7) unit cell: 8.3691(2) 8.3691(2) 8.3691(2) 90.0 90.0 90.0 V = 586.18(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) Run 6 Omega scan: (-1.000 - 24.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.904) PROFFIT INFO: signal sum: min=255.0000 max=20874476.0000 PROFFIT INFO: signal sum lp corr: min=469.0837 max=2959127.5275 PROFFIT INFO: background sum: min=619.0000 max=27145.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=12660.0000 PROFFIT INFO: num of signal pixels: min=51 max=581 PROFFIT INFO: Inet: min=750.5339 max=4734604.0000 PROFFIT INFO: sig(Inet): min=120.2540 max=47814.4414 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.84 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 68 310 666 1292 1456 2612 4262 5856 6388 Percent 0.0 0.0 1.1 4.9 10.4 20.2 22.8 40.9 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3194 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3194 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4734604- 1119279 319 1848630.01 122.31 100.00 1118986- 626139 319 849822.25 102.56 100.00 626072- 264851 319 414753.15 94.95 100.00 264400- 169691 319 203033.23 71.57 100.00 169588- 120511 319 144763.19 51.07 100.00 120504- 93887 319 105917.16 36.26 100.00 93768- 66277 319 80968.27 29.39 100.00 66195- 5636 319 37671.53 19.29 100.00 5631- 2961 319 3962.09 5.31 96.87 2959- 751 323 2128.25 3.78 55.11 ------------------------------------------------------------------------------------ 4734604- 751 3194 368705.26 53.59 95.15 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 733368.40 93.81 100.00 1.41- 1.12 319 599058.12 63.24 99.37 1.12- 0.96 319 502703.49 71.10 97.81 0.96- 0.88 319 351975.13 59.90 94.67 0.88- 0.81 319 450922.32 68.79 99.69 0.81- 0.73 319 248711.35 41.61 94.98 0.73- 0.71 319 176343.23 34.23 88.40 0.71- 0.65 319 318721.44 48.09 94.04 0.65- 0.62 319 154899.52 27.55 87.77 0.62- 0.58 323 153053.65 27.87 94.74 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 368705.26 53.59 95.15 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:40:04 2018 Sorting 3194 observations 86 unique observations with > 7.00 F2/sig(F2) 3194 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 24 546 Total number of frames 546 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3194 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 3 82 Total number of frames 82 2569 observations > 7.00 F2/sig(F2) 2569 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 3 82 Total number of frames 82 Removing 'redundancy=1' reflections Average redundancy: 27.6 (Out of 2569 removed 3 = 2566, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2566 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 3 82 Total number of frames 82 93 unique data precomputed (should be 93) 93 unique data with 2566 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.6 (Out of 2566 removed 0 = 2566, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2566 observations RMS deviation of equivalent data = 0.26000 Rint = 0.18999 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18305, wR= 0.27193 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13702, wR= 0.17723, Acormin=0.600, Acormax=1.408, Acor_av=0.982 F test: Probability=1.000, F= 1.781 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11911, wR= 0.15102, Acormin=0.565, Acormax=1.454, Acor_av=0.913 F test: Probability=1.000, F= 1.322 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10720, wR= 0.14372, Acormin=0.592, Acormax=1.551, Acor_av=0.950 F test: Probability=1.000, F= 1.231 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09130, wR= 0.12152, Acormin=0.513, Acormax=1.574, Acor_av=0.883 F test: Probability=1.000, F= 1.377 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07814, wR= 0.11000, Acormin=0.492, Acormax=1.613, Acor_av=0.898 F test: Probability=1.000, F= 1.362 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09926, wR= 0.13706, Acormin=0.603, Acormax=1.626, Acor_av=0.959 F test: Probability=0.000, F= 0.619 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08502, wR= 0.11622, Acormin=0.496, Acormax=1.606, Acor_av=0.890 F test: Probability=0.000, F= 0.843 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07534, wR= 0.10609, Acormin=0.485, Acormax=1.641, Acor_av=0.905 F test: Probability=0.952, F= 1.070 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07437, wR= 0.10307, Acormin=0.367, Acormax=1.460, Acor_av=0.803 F test: Probability=0.701, F= 1.022 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10008, wR= 0.13203, Acormin=0.452, Acormax=1.468, Acor_av=0.836 F test: Probability=0.000, F= 0.565 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08274, wR= 0.11148, Acormin=0.482, Acormax=1.601, Acor_av=0.884 F test: Probability=0.000, F= 0.826 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08340, wR= 0.11131, Acormin=0.107, Acormax=0.396, Acor_av=0.215 F test: Probability=0.000, F= 0.810 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07317, wR= 0.10034, Acormin=0.114, Acormax=0.443, Acor_av=0.245 F test: Probability=0.875, F= 1.048 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06566, wR= 0.09138, Acormin=0.133, Acormax=0.498, Acor_av=0.258 F test: Probability=1.000, F= 1.293 Final absorption model (ne=6, no=3): Rint= 0.07534, Acormin=0.485, Acormax=1.641, Acor_av=0.905 Combined refinement in use Rint: 0.19009 There are 82 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 118 pars with 7021 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26000 Using Levenberg-Marquardt: 0.00010 New wR= 0.06578 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18999 with corrections 0.05210 Rint for all data: 0.19009 with corrections 0.05231 0 observations identified as outliers and rejected Cycle 2 wR= 0.06578 Using Levenberg-Marquardt: 0.00001 New wR= 0.06117 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18999 with corrections 0.04778 Rint for all data: 0.19009 with corrections 0.04799 0 observations identified as outliers and rejected Cycle 3 wR= 0.06117 Using Levenberg-Marquardt: 0.00000 New wR= 0.06024 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18999 with corrections 0.04686 Rint for all data: 0.19009 with corrections 0.04708 0 observations identified as outliers and rejected Cycle 4 wR= 0.06024 Using Levenberg-Marquardt: 0.00000 New wR= 0.05977 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18999 with corrections 0.04643 Rint for all data: 0.19009 with corrections 0.04665 0 observations identified as outliers and rejected Cycle 5 wR= 0.05977 Using Levenberg-Marquardt: 0.00000 New wR= 0.05948 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18999 with corrections 0.04616 Rint for all data: 0.19009 with corrections 0.04637 0 observations identified as outliers and rejected Final wR= 0.05948 Final frame scales: Min= 0.6987 Max= 1.2389 Final absorption correction factors: Amin= 0.4807 Amax= 1.3541 PROFFIT INFO: Inet (after scale3 abspack): min=767.7801 max=4666164.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=105.9404 max=52008.7773 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3194 reflections read from tmp file 696 reflections are rejected (696 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 2 1 2 4 3 1 89 Initial Chi^2= 0.39305 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.90509 Current error model SIG(F2)^2 = 166.58*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 317.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 317.34*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4666164- 1087289 319 1741916.27 83.28 100.00 1083068- 610653 319 810048.25 37.26 100.00 609920- 253942 319 402321.23 39.13 100.00 253250- 153906 319 192226.32 27.76 100.00 153873- 124032 319 139149.51 18.77 100.00 123994- 87366 319 102315.50 13.29 100.00 87316- 68686 319 78454.02 11.07 100.00 68647- 4939 319 39840.13 7.71 88.40 4923- 2736 319 3632.44 2.85 21.00 2736- 768 323 2145.62 2.32 12.38 ------------------------------------------------------------------------------------ 4666164- 768 3194 350767.78 24.32 82.09 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 734460.70 58.94 98.12 1.41- 1.12 319 581337.35 37.23 88.40 1.12- 0.96 319 459865.65 31.29 83.70 0.96- 0.88 319 331673.53 22.54 83.70 0.88- 0.81 319 425448.08 25.48 90.60 0.81- 0.73 319 229118.18 15.71 69.28 0.73- 0.71 319 166128.06 12.99 77.12 0.71- 0.65 319 297172.81 17.91 90.60 0.65- 0.62 319 144419.95 10.57 68.65 0.62- 0.58 323 140687.75 10.67 70.90 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 350767.78 24.32 82.09 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 319 734460.70 58.94 98.12 4.82- 1.12 638 657899.02 48.08 93.26 4.82- 0.96 957 591887.90 42.49 90.07 4.82- 0.88 1276 526834.31 37.50 88.48 4.82- 0.81 1595 506557.06 35.10 88.90 4.82- 0.73 1914 460317.25 31.87 85.63 4.82- 0.71 2233 418290.22 29.17 84.42 4.82- 0.65 2552 403150.55 27.76 85.19 4.82- 0.62 2871 374402.70 25.85 83.35 4.82- 0.58 3194 350767.78 24.32 82.09 ------------------------------------------------------------------------------------ 4.82- 0.58 3194 350767.78 24.32 82.09 Scale applied to data: s=0.214309 (maximum obs:4666164.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.046; Rsigma 0.027: data 3194 -> merged 110 With outlier rejection... Rint 0.044; Rsigma 0.028: data 3173 -> merged 110 Rejected total: 21, method kkm 12, method Blessing 9 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585951, 4.831879 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 18.60 100.00 186 1.61 - 1.21 10 10 29.10 100.00 291 1.17 - 1.01 10 10 37.70 100.00 377 0.99 - 0.89 10 10 37.20 100.00 372 0.88 - 0.81 10 10 35.50 100.00 355 0.81 - 0.74 10 10 30.70 100.00 307 0.73 - 0.71 10 10 33.60 100.00 336 0.70 - 0.66 10 10 28.50 100.00 285 0.66 - 0.64 10 10 25.90 100.00 259 0.63 - 0.60 10 10 25.00 100.00 250 --------------------------------------------------------------- 8.37 - 0.60 100 100 30.18 100.00 3018 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:40:04 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362190 8.374076 8.370917 90.0242 90.0193 90.0272 3177 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.54 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1631 0 2131 2128 3177 N (int>3sigma) = 0 0 0 0 1631 0 2076 2069 3096 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 77.3 79.9 77.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 23.6 23.8 23.5 Lattice type: F chosen Volume: 586.18 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.97 90.06 119.93 Niggli form: a.a = 34.988 b.b = 34.996 c.c = 35.011 b.c = -17.487 a.c = -0.037 a.b = -17.460 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.084 CUBIC F-lattice R(int) = 0.043 [ 3020] Vol = 586.2 Cell: 8.362 8.374 8.371 89.98 89.98 90.03 Volume: 586.18 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.083 RHOMBOHEDRAL R-lattice R(int) = 0.048 [ 2741] Vol = 439.6 Cell: 5.916 5.915 14.498 89.97 90.05 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.083 RHOMBOHEDRAL R-lattice R(int) = 0.039 [ 873] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.498 89.97 90.05 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.061 TETRAGONAL I-lattice R(int) = 0.042 [ 2771] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.01 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.049 TETRAGONAL I-lattice R(int) = 0.042 [ 2771] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.01 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.042 [ 2718] Vol = 293.1 Cell: 5.921 8.362 5.919 89.97 89.98 89.99 Volume: 293.09 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.041 [ 2368] Vol = 293.1 Cell: 8.362 5.921 5.919 90.02 90.03 89.99 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.050 MONOCLINIC I-lattice R(int) = 0.040 [ 2371] Vol = 293.1 Cell: 5.917 5.915 8.374 89.96 90.00 89.94 Volume: 293.09 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.041 MONOCLINIC C-lattice R(int) = 0.040 [ 2381] Vol = 293.1 Cell: 8.362 8.374 5.915 89.96 134.96 90.03 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.038 [ 1718] Vol = 146.5 Cell: 5.915 5.916 5.917 119.97 90.06 119.93 Volume: 146.54 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1631 0 2128 2131 3177 N (int>3sigma) = 0 0 0 0 1631 0 2069 2076 3096 Mean intensity = 0.0 0.0 0.0 0.0 30.9 0.0 79.9 77.3 77.4 Mean int/sigma = 0.0 0.0 0.0 0.0 24.4 0.0 23.8 23.6 23.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.173 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 32 32 232 714 N I>3s 32 32 221 714 0.9 0.9 0.7 36.8 8.5 8.5 5.3 27.2 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.043 2808 Fd-3m 1 1 227 C N N N N 37 2284 0.043 2847 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362190 8.374076 8.370917 89.9758 89.9807 90.0272 ZERR 3.00 0.000611 0.000705 0.000511 0.0059 0.0055 0.0064 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3899044- 511886 706 692 27 25.6 1178057.89 55.54 0.040 0.044 505922- 118847 954 951 27 35.2 212151.59 27.45 0.051 0.071 107008- 35016 787 787 27 29.1 78671.24 11.01 0.067 0.088 10114- 1829 747 743 29 25.6 3501.45 2.80 0.169 0.229 ------------------------------------------------------------------------------------------- 3899044- 1829 3194 3173 110 28.8 340840.86 23.72 0.044 0.051 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 807 788 27 29.2 586706.42 43.73 0.038 0.039 0.016 1.01-0.78 957 957 27 35.4 334375.12 21.73 0.037 0.046 0.028 0.78-0.65 851 849 28 30.3 244835.83 15.71 0.056 0.067 0.040 0.65-0.59 579 579 28 20.7 157687.05 11.54 0.075 0.093 0.057 ------------------------------------------------------------------------------------------------------ inf-0.59 3194 3173 110 28.8 340840.86 23.72 0.044 0.051 0.028 inf-0.60 3037 3016 99 30.5 352797.90 24.46 0.043 0.049 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 788 27 27 100.0 29.2 586706.42 241.48 0.038 0.003 1.01-0.78 957 27 27 100.0 35.4 334375.12 130.62 0.037 0.005 0.78-0.65 849 28 28 100.0 30.3 244835.83 90.35 0.056 0.009 0.65-0.59 579 28 28 100.0 20.7 157687.05 60.15 0.075 0.017 -------------------------------------------------------------------------------------------- inf-0.59 3173 110 110 100.0 28.8 340840.86 134.52 0.044 0.006 inf-0.60 3016 99 99 100.0 30.5 352797.90 139.17 0.043 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:41:07 2018) ID: 2932; threads 38; handles 877; mem 520064.00 (1229512.00)kB; time: 1w 5d 0h 46m 37s MEMORY INFO: Memory PF:0.0, Ph:229.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:507.9,peak PF: 697.1, WS: 298.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:229.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:509.7,peak PF: 697.1, WS: 300.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:41:07 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00061 ) 8.37691 ( 0.00071 ) 8.37554 ( 0.00051 ) 90.02113 ( 0.00586 ) 90.03240 ( 0.00548 ) 90.03043 ( 0.00636 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:41:07 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 0.000003 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007174 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(7) 8.3755(5) 90.021(6) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.3691(2) 8.3691(2) 8.3691(2) 90.0 90.0 90.0 V = 586.18(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 453 peaks identified as outliers and rejected 446 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 446 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 446 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.984 ( 0.172) | 1.281 ( 0.701) | 1.558 ( 2.296) | 1.33- 1.09 | 45 | 1.069 ( 0.114) | 1.092 ( 0.140) | 1.111 ( 0.488) | 1.09- 0.94 | 45 | 1.056 ( 0.114) | 1.073 ( 0.140) | 1.073 ( 0.398) | 0.94- 0.84 | 45 | 1.078 ( 0.108) | 1.069 ( 0.142) | 1.142 ( 0.397) | 0.84- 0.78 | 45 | 1.104 ( 0.100) | 1.016 ( 0.119) | 1.376 ( 0.505) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.985 ( 0.124) | 1.369 ( 0.513) | 0.73- 0.69 | 45 | 1.088 ( 0.080) | 0.931 ( 0.104) | 1.361 ( 0.510) | 0.69- 0.66 | 45 | 1.068 ( 0.074) | 0.886 ( 0.097) | 1.333 ( 0.455) | 0.65- 0.62 | 45 | 1.047 ( 0.075) | 0.849 ( 0.050) | 1.363 ( 0.607) | 0.62- 0.59 | 41 | 1.026 ( 0.086) | 0.808 ( 0.035) | 1.416 ( 0.564) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 446 | 1.063 ( 0.110) | 1.001 ( 0.280) | 1.309 ( 0.880) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) UB - matrix: -0.024577 -0.079439 -0.015337 ( 0.000013 0.000011 0.000013 ) 0.072471 -0.028944 0.032942 ( 0.000014 0.000011 0.000013 ) -0.036035 -0.003353 0.076426 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007159 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007161 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3857(13) 8.3829(12) 8.3817(14) 90.069(12) 90.082(13) 89.805(12) V = 589.20(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024650 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072531 -0.028808 0.033022 ( 0.000012 0.000010 0.000011 ) -0.036123 -0.003522 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024650 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072531 -0.028808 0.033022 ( 0.000012 0.000010 0.000011 ) -0.036123 -0.003522 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) unit cell: 8.3748(12) 8.3816(11) 8.3655(12) 90.042(11) 90.079(11) 89.978(11) V = 587.20(14) unit cell: 8.3739(4) 8.3739(4) 8.3739(4) 90.0 90.0 90.0 V = 587.20(4) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024650 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072531 -0.028808 0.033022 ( 0.000012 0.000010 0.000011 ) -0.036123 -0.003522 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024650 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072531 -0.028808 0.033022 ( 0.000012 0.000010 0.000011 ) -0.036123 -0.003522 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) unit cell: 8.3748(12) 8.3816(11) 8.3655(12) 90.042(11) 90.079(11) 89.978(11) V = 587.20(14) unit cell: 8.3739(4) 8.3739(4) 8.3739(4) 90.0 90.0 90.0 V = 587.20(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.555 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.143) | 1.115 ( 0.479) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.422 ( 0.487) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.869 ( 0.062) | 1.446 ( 0.588) | 0.63- 0.59 | 45 | 1.014 ( 0.082) | 0.807 ( 0.035) | 1.312 ( 0.506) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.005 ( 0.281) | 1.320 ( 0.875) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=7, end=31, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_7.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_7.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_7.rpb PROFFITPEAK info: 373 peaks in the peak location table UB fit with 163 obs out of 181 (total:181,skipped:0) (90.06%) UB - matrix: -0.025065 -0.079614 -0.015633 ( 0.000082 0.000096 0.000043 ) 0.072663 -0.029548 0.032936 ( 0.000120 0.000141 0.000063 ) -0.035941 -0.003658 0.076567 ( 0.000049 0.000058 0.000026 ) M - matrix: 0.007200 -0.000020 0.000033 ( 0.000018 0.000013 0.000007 ) -0.000020 0.007225 -0.000009 ( 0.000013 0.000017 0.000008 ) 0.000033 -0.000009 0.007192 ( 0.000007 0.000008 0.000006 ) unit cell: 8.359(10) 8.345(10) 8.364(5) 89.93(6) 90.26(7) 89.84(10) V = 583(1) UB fit with 163 obs out of 181 (total:181,skipped:0) (90.06%) UB - matrix: -0.025065 -0.079614 -0.015633 ( 0.000082 0.000096 0.000043 ) 0.072663 -0.029548 0.032936 ( 0.000120 0.000141 0.000063 ) -0.035941 -0.003658 0.076567 ( 0.000049 0.000058 0.000026 ) M - matrix: 0.007200 -0.000020 0.000033 ( 0.000018 0.000013 0.000007 ) -0.000020 0.007225 -0.000009 ( 0.000013 0.000017 0.000008 ) 0.000033 -0.000009 0.007192 ( 0.000007 0.000008 0.000006 ) unit cell: 8.359(10) 8.345(10) 8.364(5) 89.93(6) 90.26(7) 89.84(10) V = 583(1) OTKP changes: 31 1 1 1 OTKP changes: 31 1 1 1 OTKP changes: 31 1 1 1 OTKP changes: 31 1 1 1 OTKP changes: 31 1 1 1 OTKP changes: 31 1 1 1 UB fit with 165 obs out of 181 (total:181,skipped:0) (91.16%) UB - matrix: -0.025099 -0.079632 -0.015663 ( 0.000086 0.000101 0.000045 ) 0.072663 -0.029573 0.032909 ( 0.000117 0.000137 0.000061 ) -0.035935 -0.003661 0.076579 ( 0.000046 0.000054 0.000024 ) M - matrix: 0.007201 -0.000019 0.000033 ( 0.000018 0.000013 0.000007 ) -0.000019 0.007229 -0.000006 ( 0.000013 0.000018 0.000007 ) 0.000033 -0.000006 0.007193 ( 0.000007 0.000007 0.000006 ) unit cell: 8.359(10) 8.342(10) 8.364(4) 89.95(6) 90.26(6) 89.85(10) V = 583(1) OTKP changes: 31 1 1 1 No constraint UB - matrix: -0.025106 -0.079388 -0.015603 ( 0.000084 0.000099 0.000044 ) 0.072393 -0.029485 0.032944 ( 0.000116 0.000136 0.000061 ) -0.035968 -0.003465 0.076352 ( 0.000046 0.000054 0.000024 ) M - matrix: 0.007165 -0.000017 0.000030 ( 0.000018 0.000013 0.000007 ) -0.000017 0.007184 0.000003 ( 0.000013 0.000018 0.000007 ) 0.000030 0.000003 0.007158 ( 0.000007 0.000007 0.000006 ) Constraint UB - matrix: -0.025106 -0.079388 -0.015603 ( 0.000084 0.000099 0.000044 ) 0.072393 -0.029485 0.032944 ( 0.000116 0.000136 0.000061 ) -0.035968 -0.003465 0.076352 ( 0.000046 0.000054 0.000024 ) M - matrix: 0.007140 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007140 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007140 ( 0.000000 0.000000 0.000002 ) UB fit with 165 obs out of 181 (total:181,skipped:0) (91.16%) unit cell: 8.380(10) 8.369(10) 8.384(4) 90.02(6) 90.24(6) 89.87(10) V = 588(1) unit cell: 8.3773(14) 8.3773(14) 8.3773(14) 90.0 90.0 90.0 V = 587.91(17) 181 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 30.000,31 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.039) HKL list info: 309 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025106 -0.079388 -0.015603 ( 0.000084 0.000099 0.000044 ) 0.072393 -0.029485 0.032944 ( 0.000116 0.000136 0.000061 ) -0.035968 -0.003465 0.076352 ( 0.000046 0.000054 0.000024 ) M - matrix: 0.007165 -0.000017 0.000030 ( 0.000018 0.000013 0.000007 ) -0.000017 0.007184 0.000003 ( 0.000013 0.000018 0.000007 ) 0.000030 0.000003 0.007158 ( 0.000007 0.000007 0.000006 ) Constraint UB - matrix: -0.025106 -0.079388 -0.015603 ( 0.000084 0.000099 0.000044 ) 0.072393 -0.029485 0.032944 ( 0.000116 0.000136 0.000061 ) -0.035968 -0.003465 0.076352 ( 0.000046 0.000054 0.000024 ) M - matrix: 0.007140 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007140 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007140 ( 0.000000 0.000000 0.000002 ) UB fit with 165 obs out of 181 (total:181,skipped:0) (91.16%) unit cell: 8.380(10) 8.369(10) 8.384(4) 90.02(6) 90.24(6) 89.87(10) V = 588(1) unit cell: 8.3773(14) 8.3773(14) 8.3773(14) 90.0 90.0 90.0 V = 587.91(17) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 166 obs out of 181 (total:181,skipped:0) (91.71%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=7, end=31, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_7.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_7.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_7.rpb 4 of 138 peaks identified as outliers and rejected 134 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 134 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 134 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.15- 1.61 | 13 | 0.962 ( 0.117) | 1.027 ( 0.163) | 1.032 ( 0.520) | 1.60- 1.21 | 13 | 1.025 ( 0.141) | 1.307 ( 0.672) | 1.158 ( 0.616) | 1.17- 1.02 | 13 | 1.001 ( 0.071) | 1.062 ( 0.095) | 1.027 ( 0.477) | 1.01- 0.92 | 13 | 0.956 ( 0.082) | 1.005 ( 0.101) | 0.851 ( 0.308) | 0.92- 0.84 | 13 | 1.023 ( 0.082) | 1.053 ( 0.143) | 1.134 ( 0.379) | 0.84- 0.76 | 13 | 0.985 ( 0.070) | 0.973 ( 0.126) | 1.069 ( 0.446) | 0.76- 0.72 | 13 | 0.965 ( 0.060) | 0.871 ( 0.074) | 1.251 ( 0.548) | 0.72- 0.68 | 13 | 0.961 ( 0.058) | 0.872 ( 0.055) | 1.324 ( 0.514) | 0.67- 0.64 | 13 | 0.949 ( 0.036) | 0.834 ( 0.034) | 1.256 ( 0.392) | 0.64- 0.59 | 17 | 0.919 ( 0.047) | 0.805 ( 0.029) | 1.491 ( 0.551) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.15- 0.59 | 134 | 0.973 ( 0.088) | 0.976 ( 0.270) | 1.169 ( 0.517) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) UB - matrix: -0.025178 -0.079430 -0.015390 ( 0.000059 0.000064 0.000030 ) 0.072285 -0.029243 0.032876 ( 0.000060 0.000066 0.000030 ) -0.036091 -0.003393 0.076410 ( 0.000033 0.000036 0.000017 ) M - matrix: 0.007162 0.000008 0.000006 ( 0.000009 0.000007 0.000004 ) 0.000008 0.007176 0.000002 ( 0.000007 0.000011 0.000004 ) 0.000006 0.000002 0.007156 ( 0.000004 0.000004 0.000003 ) unit cell: 8.382(5) 8.373(6) 8.385(3) 90.01(4) 90.05(4) 90.07(5) V = 588.5(6) OTKP changes: 134 1 1 1 No constraint UB - matrix: -0.025292 -0.079309 -0.015666 ( 0.000046 0.000051 0.000023 ) 0.072335 -0.029443 0.032857 ( 0.000059 0.000064 0.000030 ) -0.036077 -0.003458 0.076530 ( 0.000030 0.000033 0.000015 ) M - matrix: 0.007174 0.000001 0.000012 ( 0.000009 0.000006 0.000004 ) 0.000001 0.007169 0.000010 ( 0.000006 0.000009 0.000004 ) 0.000012 0.000010 0.007182 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: -0.025292 -0.079309 -0.015666 ( 0.000046 0.000051 0.000023 ) 0.072335 -0.029443 0.032857 ( 0.000059 0.000064 0.000030 ) -0.036077 -0.003458 0.076530 ( 0.000030 0.000033 0.000015 ) M - matrix: 0.007166 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007166 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007166 ( 0.000000 0.000000 0.000001 ) UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) unit cell: 8.375(5) 8.377(5) 8.370(2) 90.08(3) 90.10(3) 90.01(5) V = 587.2(5) unit cell: 8.3739(8) 8.3739(8) 8.3739(8) 90.0 90.0 90.0 V = 587.19(9) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 30.000,31 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.918) HKL list info: 307 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025292 -0.079309 -0.015666 ( 0.000046 0.000051 0.000023 ) 0.072335 -0.029443 0.032857 ( 0.000059 0.000064 0.000030 ) -0.036077 -0.003458 0.076530 ( 0.000030 0.000033 0.000015 ) M - matrix: 0.007174 0.000001 0.000012 ( 0.000009 0.000006 0.000004 ) 0.000001 0.007169 0.000010 ( 0.000006 0.000009 0.000004 ) 0.000012 0.000010 0.007182 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: -0.025292 -0.079309 -0.015666 ( 0.000046 0.000051 0.000023 ) 0.072335 -0.029443 0.032857 ( 0.000059 0.000064 0.000030 ) -0.036077 -0.003458 0.076530 ( 0.000030 0.000033 0.000015 ) M - matrix: 0.007166 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007166 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007166 ( 0.000000 0.000000 0.000001 ) UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) unit cell: 8.375(5) 8.377(5) 8.370(2) 90.08(3) 90.10(3) 90.01(5) V = 587.2(5) unit cell: 8.3739(8) 8.3739(8) 8.3739(8) 90.0 90.0 90.0 V = 587.19(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=7, end=31, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_7.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_7.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_7.rpb 2 of 136 peaks identified as outliers and rejected 134 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 134 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 134 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 1.61 | 13 | 0.963 ( 0.118) | 1.028 ( 0.163) | 1.030 ( 0.517) | 1.61- 1.26 | 13 | 1.003 ( 0.140) | 1.229 ( 0.589) | 1.020 ( 0.501) | 1.21- 1.09 | 13 | 1.008 ( 0.072) | 1.081 ( 0.114) | 1.126 ( 0.609) | 1.02- 0.92 | 13 | 1.007 ( 0.097) | 1.091 ( 0.163) | 0.861 ( 0.327) | 0.92- 0.84 | 13 | 0.999 ( 0.084) | 1.013 ( 0.141) | 1.115 ( 0.450) | 0.84- 0.78 | 13 | 0.990 ( 0.070) | 0.983 ( 0.129) | 1.124 ( 0.439) | 0.76- 0.72 | 13 | 0.965 ( 0.061) | 0.880 ( 0.081) | 1.260 ( 0.534) | 0.72- 0.68 | 13 | 0.957 ( 0.055) | 0.875 ( 0.055) | 1.235 ( 0.482) | 0.67- 0.64 | 13 | 0.951 ( 0.037) | 0.837 ( 0.034) | 1.258 ( 0.392) | 0.64- 0.59 | 17 | 0.921 ( 0.047) | 0.807 ( 0.031) | 1.565 ( 0.556) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.12- 0.59 | 134 | 0.975 ( 0.088) | 0.977 ( 0.247) | 1.172 ( 0.524) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-13.3 | 239 | 1.117 ( 0.130) | 1.234 ( 0.472) | 1.256 ( 1.124) | 13.3-18.9 | 239 | 1.077 ( 0.053) | 1.131 ( 0.272) | 1.178 ( 0.515) | 19.0-23.2 | 239 | 1.065 ( 0.069) | 1.135 ( 0.368) | 1.155 ( 0.526) | 23.2-27.2 | 239 | 1.031 ( 0.074) | 1.063 ( 0.247) | 1.165 ( 0.551) | 27.3-30.8 | 239 | 1.007 ( 0.076) | 1.005 ( 0.210) | 1.177 ( 0.496) | 30.8-33.9 | 239 | 0.979 ( 0.078) | 0.928 ( 0.113) | 1.211 ( 0.512) | 33.9-37.0 | 239 | 0.958 ( 0.075) | 0.901 ( 0.105) | 1.176 ( 0.484) | 37.0-39.7 | 239 | 0.941 ( 0.084) | 0.868 ( 0.130) | 1.222 ( 0.555) | 39.7-42.8 | 239 | 0.922 ( 0.079) | 0.837 ( 0.091) | 1.215 ( 0.555) | 42.8-49.9 | 234 | 0.925 ( 0.084) | 0.810 ( 0.063) | 1.144 ( 0.469) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2385 | 1.002 ( 0.105) | 0.992 ( 0.279) | 1.190 ( 0.608) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0021 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 23819788 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 15:41:37 2018 PROFFITMAIN - Started at Tue Mar 27 15:41:37 2018 OTKP changes: 2379 2 4 6 OTKP changes: 2379 2 4 6 No constraint UB - matrix: -0.025031 -0.079526 -0.015579 ( 0.000006 0.000007 0.000006 ) 0.072515 -0.029192 0.032938 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003599 0.076550 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007198 0.000004 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007189 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000002 0.007187 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025031 -0.079526 -0.015579 ( 0.000006 0.000007 0.000006 ) 0.072515 -0.029192 0.032938 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003599 0.076550 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) UB fit with 2382 obs out of 2385 (total:2385,skipped:0) (99.87%) unit cell: 8.3605(5) 8.3653(6) 8.3665(5) 90.015(5) 90.039(5) 90.033(6) V = 585.14(7) unit cell: 8.36409(15) 8.36409(15) 8.36409(15) 90.0 90.0 90.0 V = 585.136(19) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036112 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.044(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3661(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3741(4) 8.3741(4) 8.3741(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3661(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3741(4) 8.3741(4) 8.3741(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024640 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3661(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3741(4) 8.3741(4) 8.3741(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024861 -0.079568 -0.015654 ( 0.000013 0.000015 0.000011 ) 0.072453 -0.029196 0.032946 ( 0.000016 0.000018 0.000013 ) -0.036281 -0.003652 0.076380 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000005 0.000005 ( 0.000003 0.000002 0.000001 ) -0.000005 0.007197 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000005 0.000005 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3686(15) 8.3610(15) 8.3800(10) 90.038(12) 90.040(12) 89.962(14) V = 586.34(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024987 -0.079526 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072499 -0.029263 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036259 -0.003623 0.076513 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000003 0.000006 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000010 0.007184 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3620(11) 8.3628(14) 8.3687(11) 89.922(12) 90.045(11) 89.976(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3575(14) 8.3628(11) 89.935(12) 90.003(11) 89.963(12) V = 584.01(15) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.01(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) HKL list info: 787 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3575(14) 8.3628(11) 89.935(12) 90.003(11) 89.963(12) V = 584.01(15) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.01(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007203 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079573 -0.015476 ( 0.000016 0.000014 0.000012 ) 0.072543 -0.029297 0.032983 ( 0.000011 0.000010 0.000008 ) -0.036290 -0.003568 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3560(11) 8.3575(14) 8.3628(11) 89.935(12) 90.003(11) 89.963(12) V = 584.01(15) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.01(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025023 -0.079533 -0.015717 ( 0.000008 0.000013 0.000012 ) 0.072409 -0.029343 0.032916 ( 0.000008 0.000014 0.000014 ) -0.036195 -0.003661 0.076524 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007179 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000004 0.007186 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3712(11) 8.3593(12) 8.3671(11) 90.031(11) 90.055(11) 89.983(11) V = 585.51(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3666(10) 8.3559(12) 8.3596(11) 89.995(11) 90.023(10) 90.026(11) V = 584.43(13) unit cell: 8.3607(3) 8.3607(3) 8.3607(3) 90.0 90.0 90.0 V = 584.43(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3666(10) 8.3559(12) 8.3596(11) 89.995(11) 90.023(10) 90.026(11) V = 584.43(13) unit cell: 8.3607(3) 8.3607(3) 8.3607(3) 90.0 90.0 90.0 V = 584.43(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007187 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007199 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025084 -0.079557 -0.015726 ( 0.000008 0.000013 0.000013 ) 0.072394 -0.029373 0.032982 ( 0.000008 0.000014 0.000013 ) -0.036294 -0.003695 0.076577 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3666(10) 8.3559(12) 8.3596(11) 89.995(11) 90.023(10) 90.026(11) V = 584.43(13) unit cell: 8.3607(3) 8.3607(3) 8.3607(3) 90.0 90.0 90.0 V = 584.43(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025241 -0.079445 -0.015765 ( 0.000011 0.000016 0.000017 ) 0.072355 -0.029415 0.032793 ( 0.000008 0.000011 0.000012 ) -0.036255 -0.003616 0.076600 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007187 0.000008 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007190 0.000011 ( 0.000001 0.000003 0.000002 ) -0.000006 0.000011 0.007192 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3669(10) 8.3651(14) 8.3641(11) 90.086(12) 89.949(10) 90.064(12) V = 585.40(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3602(10) 8.3611(14) 8.3567(11) 90.050(12) 89.991(10) 90.063(11) V = 584.14(14) unit cell: 8.3593(3) 8.3593(3) 8.3593(3) 90.0 90.0 90.0 V = 584.14(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3602(10) 8.3611(14) 8.3567(11) 90.050(12) 89.991(10) 90.063(11) V = 584.14(14) unit cell: 8.3593(3) 8.3593(3) 8.3593(3) 90.0 90.0 90.0 V = 584.14(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007198 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007204 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025254 -0.079486 -0.015745 ( 0.000011 0.000015 0.000017 ) 0.072458 -0.029419 0.032804 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003653 0.076682 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3602(10) 8.3611(14) 8.3567(11) 90.050(12) 89.991(10) 90.063(11) V = 584.14(14) unit cell: 8.3593(3) 8.3593(3) 8.3593(3) 90.0 90.0 90.0 V = 584.14(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) UB - matrix: -0.025241 -0.079424 -0.015591 ( 0.000050 0.000055 0.000025 ) 0.072383 -0.029417 0.032836 ( 0.000058 0.000063 0.000029 ) -0.036082 -0.003543 0.076574 ( 0.000033 0.000036 0.000017 ) M - matrix: 0.007178 0.000003 0.000007 ( 0.000009 0.000007 0.000004 ) 0.000003 0.007186 0.000001 ( 0.000007 0.000009 0.000004 ) 0.000007 0.000001 0.007185 ( 0.000004 0.000004 0.000003 ) unit cell: 8.372(5) 8.367(5) 8.368(3) 90.01(4) 90.06(3) 90.03(5) V = 586.2(5) OTKP changes: 134 1 1 1 No constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007176 0.000001 0.000011 ( 0.000009 0.000006 0.000004 ) 0.000001 0.007173 0.000010 ( 0.000006 0.000009 0.000004 ) 0.000011 0.000010 0.007185 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007170 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007170 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007170 ( 0.000000 0.000000 0.000001 ) UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) unit cell: 8.373(5) 8.375(5) 8.368(3) 90.08(3) 90.09(3) 90.01(5) V = 586.8(5) unit cell: 8.3721(8) 8.3721(8) 8.3721(8) 90.0 90.0 90.0 V = 586.82(9) Run 6 Omega scan: (-1.000 - 30.000,31 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.903) HKL list info: 299 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007176 0.000001 0.000011 ( 0.000009 0.000006 0.000004 ) 0.000001 0.007173 0.000010 ( 0.000006 0.000009 0.000004 ) 0.000011 0.000010 0.007185 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007170 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007170 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007170 ( 0.000000 0.000000 0.000001 ) UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) unit cell: 8.373(5) 8.375(5) 8.368(3) 90.08(3) 90.09(3) 90.01(5) V = 586.8(5) unit cell: 8.3721(8) 8.3721(8) 8.3721(8) 90.0 90.0 90.0 V = 586.82(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007176 0.000001 0.000011 ( 0.000009 0.000006 0.000004 ) 0.000001 0.007173 0.000010 ( 0.000006 0.000009 0.000004 ) 0.000011 0.000010 0.007185 ( 0.000004 0.000004 0.000003 ) Constraint UB - matrix: -0.025288 -0.079333 -0.015669 ( 0.000047 0.000051 0.000023 ) 0.072350 -0.029442 0.032853 ( 0.000058 0.000063 0.000029 ) -0.036084 -0.003471 0.076551 ( 0.000031 0.000034 0.000016 ) M - matrix: 0.007170 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007170 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007170 ( 0.000000 0.000000 0.000001 ) UB fit with 134 obs out of 134 (total:134,skipped:0) (100.00%) unit cell: 8.373(5) 8.375(5) 8.368(3) 90.08(3) 90.09(3) 90.01(5) V = 586.8(5) unit cell: 8.3721(8) 8.3721(8) 8.3721(8) 90.0 90.0 90.0 V = 586.82(9) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=31, width=1.000 - Required frames: #=25, start=26, end=50, - Adjusted required frames (end): #=25, start=7, end=31, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_7.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_7.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_7.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025013 -0.079450 -0.015552 ( 0.000006 0.000007 0.000007 ) 0.072504 -0.029152 0.032900 ( 0.000006 0.000007 0.000007 ) -0.036221 -0.003574 0.076521 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025013 -0.079450 -0.015552 ( 0.000006 0.000007 0.000007 ) 0.072504 -0.029152 0.032900 ( 0.000006 0.000007 0.000007 ) -0.036221 -0.003574 0.076521 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) UB fit with 2382 obs out of 2385 (total:2385,skipped:0) (99.87%) unit cell: 8.3624(6) 8.3737(7) 8.3709(5) 90.024(6) 90.022(5) 90.025(6) V = 586.17(7) unit cell: 8.3690(2) 8.3690(2) 8.3690(2) 90.0 90.0 90.0 V = 586.17(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 69 reflections under beam stop or inside a detector rejection region 21 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3225 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:41:45 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) Run 6 Omega scan: (-1.000 - 30.000,31 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.903) PROFFIT INFO: signal sum: min=258.0000 max=20874476.0000 PROFFIT INFO: signal sum lp corr: min=469.8829 max=2961541.4864 PROFFIT INFO: background sum: min=619.0000 max=27145.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=12660.0000 PROFFIT INFO: num of signal pixels: min=51 max=575 PROFFIT INFO: Inet: min=751.8126 max=4738466.5000 PROFFIT INFO: sig(Inet): min=120.3231 max=47814.4414 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.95 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 37 158 337 655 739 1328 2157 2959 3225 Percent 0.0 0.0 1.1 4.9 10.4 20.3 22.9 41.2 66.9 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3225 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3225 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4738467- 1119924 322 1851490.89 122.18 100.00 1119847- 623089 322 846831.78 102.28 100.00 622811- 263871 322 411343.76 94.76 100.00 263628- 169415 322 202048.03 71.29 100.00 169376- 119592 322 143976.97 51.16 100.00 119377- 93251 322 105389.72 35.77 100.00 93225- 65741 322 80353.30 29.19 100.00 65719- 5570 322 37114.79 19.13 100.00 5549- 2958 322 3931.60 5.26 97.20 2949- 752 327 2118.86 3.77 54.43 ------------------------------------------------------------------------------------ 4738467- 752 3225 367892.00 53.40 95.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 738319.04 93.68 100.00 1.41- 1.12 322 607199.21 63.50 99.38 1.12- 0.96 322 492055.61 70.49 97.83 0.96- 0.88 322 350195.47 59.77 94.41 0.88- 0.81 322 449631.51 68.60 99.38 0.81- 0.73 322 245427.09 41.05 94.72 0.73- 0.71 322 176339.04 34.15 87.89 0.71- 0.65 322 316396.48 47.89 94.72 0.65- 0.62 322 153767.55 27.42 87.89 0.62- 0.58 327 152926.97 27.87 94.80 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 367892.00 53.40 95.10 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:41:45 2018 Sorting 3225 observations 119 unique observations with > 7.00 F2/sig(F2) 3225 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 29 551 Total number of frames 551 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3225 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 5 112 Total number of frames 112 2590 observations > 7.00 F2/sig(F2) 2590 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 5 112 Total number of frames 112 Removing 'redundancy=1' reflections Average redundancy: 20.3 (Out of 2590 removed 6 = 2584, unique = 127) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2584 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 5 112 Total number of frames 112 127 unique data precomputed (should be 127) 127 unique data with 2584 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.3 (Out of 2584 removed 0 = 2584, unique = 127) 127 unique data precomputed (should be 127) 127 unique data with 2584 observations RMS deviation of equivalent data = 0.25980 Rint = 0.19063 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18320, wR= 0.27003 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13665, wR= 0.17543, Acormin=0.600, Acormax=1.409, Acor_av=0.982 F test: Probability=1.000, F= 1.794 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11898, wR= 0.15045, Acormin=0.564, Acormax=1.451, Acor_av=0.913 F test: Probability=1.000, F= 1.317 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10689, wR= 0.14210, Acormin=0.592, Acormax=1.549, Acor_av=0.950 F test: Probability=1.000, F= 1.236 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09124, wR= 0.12070, Acormin=0.518, Acormax=1.573, Acor_av=0.884 F test: Probability=1.000, F= 1.371 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07878, wR= 0.10956, Acormin=0.497, Acormax=1.613, Acor_av=0.899 F test: Probability=1.000, F= 1.337 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09955, wR= 0.13573, Acormin=0.607, Acormax=1.619, Acor_av=0.959 F test: Probability=0.000, F= 0.625 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08543, wR= 0.11563, Acormin=0.498, Acormax=1.605, Acor_av=0.891 F test: Probability=0.000, F= 0.848 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07591, wR= 0.10587, Acormin=0.487, Acormax=1.642, Acor_av=0.906 F test: Probability=0.955, F= 1.071 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07460, wR= 0.10252, Acormin=0.370, Acormax=1.473, Acor_av=0.811 F test: Probability=0.771, F= 1.031 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09978, wR= 0.13052, Acormin=0.443, Acormax=1.468, Acor_av=0.836 F test: Probability=0.000, F= 0.577 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08340, wR= 0.11098, Acormin=0.483, Acormax=1.603, Acor_av=0.882 F test: Probability=0.000, F= 0.825 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08351, wR= 0.11059, Acormin=0.109, Acormax=0.401, Acor_av=0.219 F test: Probability=0.000, F= 0.820 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07309, wR= 0.09972, Acormin=0.114, Acormax=0.450, Acor_av=0.249 F test: Probability=0.942, F= 1.066 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06626, wR= 0.09116, Acormin=0.135, Acormax=0.507, Acor_av=0.263 F test: Probability=1.000, F= 1.289 Final absorption model (ne=6, no=3): Rint= 0.07591, Acormin=0.487, Acormax=1.642, Acor_av=0.906 Combined refinement in use Rint: 0.19072 There are 112 active scales (one needs to be fixed) Refinement control: frame scale #51 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 148 pars with 11026 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25980 Using Levenberg-Marquardt: 0.00010 New wR= 0.06229 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19063 with corrections 0.04919 Rint for all data: 0.19072 with corrections 0.04942 0 observations identified as outliers and rejected Cycle 2 wR= 0.06229 Using Levenberg-Marquardt: 0.00001 New wR= 0.05886 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19063 with corrections 0.04629 Rint for all data: 0.19072 with corrections 0.04651 0 observations identified as outliers and rejected Cycle 3 wR= 0.05886 Using Levenberg-Marquardt: 0.00000 New wR= 0.05820 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19063 with corrections 0.04572 Rint for all data: 0.19072 with corrections 0.04595 0 observations identified as outliers and rejected Cycle 4 wR= 0.05820 Using Levenberg-Marquardt: 0.00000 New wR= 0.05786 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19063 with corrections 0.04542 Rint for all data: 0.19072 with corrections 0.04565 0 observations identified as outliers and rejected Cycle 5 wR= 0.05786 Using Levenberg-Marquardt: 0.00000 New wR= 0.05766 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19063 with corrections 0.04525 Rint for all data: 0.19072 with corrections 0.04548 0 observations identified as outliers and rejected Final wR= 0.05766 Final frame scales: Min= 0.6512 Max= 1.1953 Final absorption correction factors: Amin= 0.4831 Amax= 1.3889 PROFFIT INFO: Inet (after scale3 abspack): min=766.2663 max=4615152.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=105.3940 max=52486.4648 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3225 reflections read from tmp file 676 reflections are rejected (674 as outliers, 2 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 4 4 3 3 5 5 9 117 Initial Chi^2= 0.41860 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94046 Current error model SIG(F2)^2 = 155.81*I_RAW + 0.00*I_BACK+(0.01553*)^2 Cycle 2, Chi^2= 1.00761 Current error model SIG(F2)^2 = 109.73*I_RAW + 0.00*I_BACK+(0.02155*)^2 Cycle 3, Chi^2= 1.00026 Current error model SIG(F2)^2 = 115.73*I_RAW + 0.00*I_BACK+(0.02045*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 115.50*I_RAW + 0.00*I_BACK+(0.02051*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 115.50*I_RAW + 0.00*I_BACK+(0.02051*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4615153- 1076953 322 1745612.81 45.29 100.00 1074412- 605218 322 805900.40 37.88 100.00 605135- 253834 322 399402.49 36.61 100.00 253770- 153917 322 190838.21 31.81 100.00 153897- 123779 322 138521.54 25.69 100.00 123617- 86961 322 101540.39 19.81 100.00 86889- 68172 322 78167.77 16.98 100.00 68033- 4887 322 39235.41 12.14 100.00 4828- 2741 322 3604.19 4.63 96.27 2737- 766 327 2136.70 3.81 75.54 ------------------------------------------------------------------------------------ 4615153- 766 3225 349955.90 23.44 97.15 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 739592.54 37.06 100.00 1.41- 1.12 322 591587.14 29.04 99.38 1.12- 0.96 322 447836.93 27.91 98.76 0.96- 0.88 322 329189.21 24.04 97.20 0.88- 0.81 322 424107.96 27.48 99.69 0.81- 0.73 322 225982.56 18.97 96.27 0.73- 0.71 322 166100.91 17.48 92.55 0.71- 0.65 322 294835.20 22.64 97.83 0.65- 0.62 322 142909.17 14.69 92.86 0.62- 0.58 327 140667.19 15.18 96.94 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 349955.90 23.44 97.15 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 739592.54 37.06 100.00 4.82- 1.12 644 665589.84 33.05 99.69 4.82- 0.96 966 593005.54 31.34 99.38 4.82- 0.88 1288 527051.46 29.51 98.84 4.82- 0.81 1610 506462.76 29.11 99.01 4.82- 0.73 1932 459716.06 27.42 98.55 4.82- 0.71 2254 417771.04 26.00 97.69 4.82- 0.65 2576 402404.06 25.58 97.71 4.82- 0.62 2898 373571.29 24.37 97.17 4.82- 0.58 3225 349955.90 23.44 97.15 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 349955.90 23.44 97.15 Scale applied to data: s=0.216677 (maximum obs:4615152.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.045; Rsigma 0.028: data 3225 -> merged 157 With outlier rejection... Rint 0.044; Rsigma 0.028: data 3203 -> merged 157 Rejected total: 22, method kkm 21, method Blessing 1 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585949, 4.831862 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.48 14 14 18.14 100.00 254 1.41 - 1.12 14 14 26.29 100.00 368 1.12 - 0.97 14 14 26.29 100.00 368 0.96 - 0.84 14 14 28.21 100.00 395 0.84 - 0.78 14 14 21.57 100.00 302 0.78 - 0.73 14 14 22.71 100.00 318 0.73 - 0.69 14 14 21.07 100.00 295 0.69 - 0.66 14 14 18.21 100.00 255 0.65 - 0.63 14 14 18.71 100.00 262 0.63 - 0.60 14 14 16.57 100.00 232 --------------------------------------------------------------- 8.38 - 0.60 140 140 21.78 100.00 3049 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:41:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362428 8.373725 8.370946 90.0239 90.0215 90.0252 3203 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1646 0 2148 2147 3203 N (int>3sigma) = 0 0 0 0 1646 0 2087 2081 3111 Mean intensity = 0.0 0.0 0.0 0.0 30.3 0.0 74.6 77.4 75.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 23.5 23.7 23.4 Lattice type: F chosen Volume: 586.17 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.97 90.06 119.93 Niggli form: a.a = 34.988 b.b = 34.997 c.c = 35.014 b.c = -17.489 a.c = -0.036 a.b = -17.461 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.082 CUBIC F-lattice R(int) = 0.044 [ 3046] Vol = 586.2 Cell: 8.362 8.374 8.371 89.98 89.98 90.03 Volume: 586.17 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.049 [ 2767] Vol = 439.6 Cell: 5.916 5.915 14.498 89.97 90.04 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 882] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.498 89.97 90.04 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.058 TETRAGONAL I-lattice R(int) = 0.042 [ 2797] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.00 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.047 TETRAGONAL I-lattice R(int) = 0.042 [ 2797] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.00 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.031 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 2743] Vol = 293.1 Cell: 5.921 8.362 5.919 89.97 89.98 90.00 Volume: 293.09 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.041 [ 2393] Vol = 293.1 Cell: 8.362 5.921 5.919 90.02 90.03 90.00 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.048 MONOCLINIC I-lattice R(int) = 0.040 [ 2397] Vol = 293.1 Cell: 5.917 5.915 8.374 89.97 90.00 89.94 Volume: 293.09 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.039 MONOCLINIC C-lattice R(int) = 0.041 [ 2408] Vol = 293.1 Cell: 8.362 8.374 5.915 89.97 134.96 90.03 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.037 [ 1743] Vol = 146.5 Cell: 5.915 5.916 5.917 119.97 90.06 119.93 Volume: 146.54 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1646 0 2147 2148 3203 N (int>3sigma) = 0 0 0 0 1646 0 2081 2087 3111 Mean intensity = 0.0 0.0 0.0 0.0 30.3 0.0 77.4 74.6 75.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 23.7 23.5 23.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.176 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 31 31 232 722 N I>3s 31 31 220 722 0.9 0.9 0.7 36.0 8.5 8.5 5.3 27.0 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.044 2834 Fd-3m 1 1 227 C N N N N 37 2284 0.044 2873 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362428 8.373725 8.370946 89.9761 89.9785 90.0252 ZERR 3.00 0.000612 0.000700 0.000511 0.0058 0.0055 0.0063 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3888459- 747213 526 521 26 20.0 1397052.02 42.84 0.038 0.045 742653- 221710 498 496 26 19.1 444018.28 36.62 0.059 0.076 219843- 97526 747 747 26 28.7 147588.44 26.49 0.042 0.054 95204- 69750 519 516 26 19.8 82048.82 17.20 0.066 0.082 64688- 3582 419 415 26 16.0 26016.78 9.16 0.082 0.108 3344- 1701 516 508 27 18.8 2605.48 4.20 0.180 0.227 ------------------------------------------------------------------------------------------- 3888459- 1701 3225 3203 157 20.4 347425.38 23.44 0.044 0.055 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 599 586 26 22.5 591963.40 32.36 0.044 0.051 0.023 1.12-0.88 709 707 26 27.2 455273.16 27.28 0.033 0.039 0.025 0.85-0.75 601 600 26 23.1 323860.74 22.83 0.040 0.050 0.029 0.74-0.68 523 521 26 20.0 256416.64 20.55 0.055 0.065 0.033 0.67-0.63 497 496 26 19.1 147092.40 16.14 0.070 0.087 0.041 0.62-0.59 296 293 27 10.9 147329.20 15.06 0.071 0.082 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3225 3203 157 20.4 347425.38 23.44 0.044 0.055 0.028 inf-0.60 3067 3047 139 21.9 359691.47 23.93 0.044 0.053 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 586 26 26 100.0 22.5 591963.40 168.30 0.044 0.006 1.12-0.88 707 26 26 100.0 27.2 455273.16 145.24 0.033 0.005 0.85-0.75 600 26 26 100.0 23.1 323860.74 116.29 0.040 0.006 0.74-0.68 521 26 26 100.0 20.0 256416.64 94.41 0.055 0.008 0.67-0.63 496 26 26 100.0 19.1 147092.40 69.86 0.070 0.010 0.62-0.59 293 27 27 100.0 10.9 147329.20 57.84 0.071 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3203 157 157 100.0 20.4 347425.38 116.10 0.044 0.007 inf-0.60 3047 139 139 100.0 21.9 359691.47 119.57 0.044 0.007 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025013 -0.079450 -0.015552 ( 0.000006 0.000007 0.000007 ) 0.072504 -0.029152 0.032900 ( 0.000006 0.000007 0.000007 ) -0.036221 -0.003574 0.076521 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025013 -0.079450 -0.015552 ( 0.000006 0.000007 0.000007 ) 0.072504 -0.029152 0.032900 ( 0.000006 0.000007 0.000007 ) -0.036221 -0.003574 0.076521 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3624(6) 8.3737(7) 8.3709(5) 90.024(6) 90.022(5) 90.025(6) V = 586.17(7) unit cell: 8.3690(2) 8.3690(2) 8.3690(2) 90.0 90.0 90.0 V = 586.17(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.763) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.763) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.763) Run 6 Omega scan: (-1.000 - 30.000,31 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.903) PROFFIT INFO: signal sum: min=258.0000 max=20874476.0000 PROFFIT INFO: signal sum lp corr: min=469.8829 max=2961541.4864 PROFFIT INFO: background sum: min=619.0000 max=27145.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=12660.0000 PROFFIT INFO: num of signal pixels: min=51 max=575 PROFFIT INFO: Inet: min=751.8126 max=4738466.5000 PROFFIT INFO: sig(Inet): min=120.3231 max=47814.4414 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.95 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 74 316 674 1310 1478 2656 4314 5918 6450 Percent 0.0 0.0 1.1 4.9 10.4 20.3 22.9 41.2 66.9 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3225 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3225 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4738467- 1119924 322 1851490.89 122.18 100.00 1119847- 623089 322 846831.78 102.28 100.00 622811- 263871 322 411343.76 94.76 100.00 263628- 169415 322 202048.03 71.29 100.00 169376- 119592 322 143976.97 51.16 100.00 119377- 93251 322 105389.72 35.77 100.00 93225- 65741 322 80353.30 29.19 100.00 65719- 5570 322 37114.79 19.13 100.00 5549- 2958 322 3931.60 5.26 97.20 2949- 752 327 2118.86 3.77 54.43 ------------------------------------------------------------------------------------ 4738467- 752 3225 367892.00 53.40 95.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 738319.04 93.68 100.00 1.41- 1.12 322 607199.21 63.50 99.38 1.12- 0.96 322 492055.61 70.49 97.83 0.96- 0.88 322 350195.47 59.77 94.41 0.88- 0.81 322 449631.51 68.60 99.38 0.81- 0.73 322 245427.09 41.05 94.72 0.73- 0.71 322 176339.04 34.15 87.89 0.71- 0.65 322 316396.48 47.89 94.72 0.65- 0.62 322 153767.55 27.42 87.89 0.62- 0.58 327 152926.97 27.87 94.80 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 367892.00 53.40 95.10 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:41:46 2018 Sorting 3225 observations 86 unique observations with > 7.00 F2/sig(F2) 3225 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 29 551 Total number of frames 551 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3225 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 4 83 Total number of frames 83 2590 observations > 7.00 F2/sig(F2) 2590 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 4 83 Total number of frames 83 Removing 'redundancy=1' reflections Average redundancy: 27.8 (Out of 2590 removed 3 = 2587, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2587 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 4 83 Total number of frames 83 93 unique data precomputed (should be 93) 93 unique data with 2587 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.8 (Out of 2587 removed 0 = 2587, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2587 observations RMS deviation of equivalent data = 0.26019 Rint = 0.19091 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18413, wR= 0.27208 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13739, wR= 0.17723, Acormin=0.600, Acormax=1.410, Acor_av=0.983 F test: Probability=1.000, F= 1.793 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11980, wR= 0.15129, Acormin=0.563, Acormax=1.454, Acor_av=0.912 F test: Probability=1.000, F= 1.314 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10774, wR= 0.14371, Acormin=0.594, Acormax=1.554, Acor_av=0.952 F test: Probability=1.000, F= 1.233 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09167, wR= 0.12159, Acormin=0.513, Acormax=1.574, Acor_av=0.884 F test: Probability=1.000, F= 1.380 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07892, wR= 0.11015, Acormin=0.493, Acormax=1.614, Acor_av=0.900 F test: Probability=1.000, F= 1.346 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09995, wR= 0.13710, Acormin=0.604, Acormax=1.629, Acor_av=0.961 F test: Probability=0.000, F= 0.623 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08576, wR= 0.11631, Acormin=0.496, Acormax=1.606, Acor_av=0.891 F test: Probability=0.000, F= 0.845 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07600, wR= 0.10622, Acormin=0.487, Acormax=1.642, Acor_av=0.907 F test: Probability=0.959, F= 1.073 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07481, wR= 0.10274, Acormin=0.372, Acormax=1.473, Acor_av=0.812 F test: Probability=0.748, F= 1.027 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10069, wR= 0.13202, Acormin=0.452, Acormax=1.468, Acor_av=0.836 F test: Probability=0.000, F= 0.568 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08348, wR= 0.11159, Acormin=0.483, Acormax=1.600, Acor_av=0.884 F test: Probability=0.000, F= 0.825 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08392, wR= 0.11141, Acormin=0.108, Acormax=0.397, Acor_av=0.215 F test: Probability=0.000, F= 0.815 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07377, wR= 0.10042, Acormin=0.114, Acormax=0.443, Acor_av=0.245 F test: Probability=0.883, F= 1.049 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06650, wR= 0.09160, Acormin=0.133, Acormax=0.500, Acor_av=0.259 F test: Probability=1.000, F= 1.283 Final absorption model (ne=6, no=3): Rint= 0.07600, Acormin=0.487, Acormax=1.642, Acor_av=0.907 Combined refinement in use Rint: 0.19101 There are 83 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 119 pars with 7140 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26019 Using Levenberg-Marquardt: 0.00010 New wR= 0.06594 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19091 with corrections 0.05327 Rint for all data: 0.19101 with corrections 0.05349 0 observations identified as outliers and rejected Cycle 2 wR= 0.06594 Using Levenberg-Marquardt: 0.00001 New wR= 0.06128 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19091 with corrections 0.04891 Rint for all data: 0.19101 with corrections 0.04913 0 observations identified as outliers and rejected Cycle 3 wR= 0.06128 Using Levenberg-Marquardt: 0.00000 New wR= 0.06034 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19091 with corrections 0.04794 Rint for all data: 0.19101 with corrections 0.04817 0 observations identified as outliers and rejected Cycle 4 wR= 0.06034 Using Levenberg-Marquardt: 0.00000 New wR= 0.05990 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19091 with corrections 0.04749 Rint for all data: 0.19101 with corrections 0.04771 0 observations identified as outliers and rejected Cycle 5 wR= 0.05990 Using Levenberg-Marquardt: 0.00000 New wR= 0.05964 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19091 with corrections 0.04722 Rint for all data: 0.19101 with corrections 0.04744 0 observations identified as outliers and rejected Final wR= 0.05964 Final frame scales: Min= 0.6990 Max= 1.2388 Final absorption correction factors: Amin= 0.4717 Amax= 1.3802 PROFFIT INFO: Inet (after scale3 abspack): min=759.9886 max=4668102.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=105.2515 max=52172.7930 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3225 reflections read from tmp file 729 reflections are rejected (729 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 2 2 3 3 2 4 87 Initial Chi^2= 0.39225 Negative value encountered! Resetting parameters to initial values... Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 2.05227 Current error model SIG(F2)^2 = 163.69*I_RAW + 0.00*I_BACK+(0.00000*)^2 Cycle 2, Chi^2= 1.00000 Current error model SIG(F2)^2 = 335.94*I_RAW + 0.00*I_BACK+(0.00000*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 335.94*I_RAW + 0.00*I_BACK+(0.00000*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4668103- 1073575 322 1745110.16 81.09 100.00 1071115- 607427 322 807210.34 36.17 100.00 607354- 253035 322 399248.66 37.87 100.00 252469- 153791 322 191097.22 26.91 100.00 153699- 123773 322 138600.72 18.21 100.00 123753- 86934 322 101593.81 12.78 100.00 86918- 68544 322 78129.73 10.71 100.00 68478- 4893 322 39233.09 7.45 86.34 4856- 2719 322 3606.16 2.74 18.63 2715- 760 327 2136.39 2.25 10.40 ------------------------------------------------------------------------------------ 4668103- 760 3225 350056.38 23.59 81.43 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 738942.40 57.39 98.14 1.41- 1.12 322 591100.15 36.51 86.65 1.12- 0.96 322 447975.09 29.99 83.54 0.96- 0.88 322 329562.22 21.86 83.54 0.88- 0.81 322 424596.92 24.70 89.75 0.81- 0.73 322 226268.33 15.07 68.63 0.73- 0.71 322 166373.19 12.60 75.16 0.71- 0.65 322 294871.50 17.34 90.68 0.65- 0.62 322 143386.80 10.23 68.32 0.62- 0.58 327 140737.50 10.37 70.03 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 350056.38 23.59 81.43 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 322 738942.40 57.39 98.14 4.82- 1.12 644 665021.27 46.95 92.39 4.82- 0.96 966 592672.54 41.30 89.44 4.82- 0.88 1288 526894.96 36.44 87.97 4.82- 0.81 1610 506435.35 34.09 88.32 4.82- 0.73 1932 459740.85 30.92 85.04 4.82- 0.71 2254 417831.18 28.30 83.63 4.82- 0.65 2576 402461.22 26.93 84.51 4.82- 0.62 2898 373675.18 25.08 82.71 4.82- 0.58 3225 350056.38 23.59 81.43 ------------------------------------------------------------------------------------ 4.82- 0.58 3225 350056.38 23.59 81.43 Scale applied to data: s=0.214220 (maximum obs:4668102.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.028: data 3225 -> merged 110 With outlier rejection... Rint 0.045; Rsigma 0.028: data 3203 -> merged 110 Rejected total: 22, method kkm 13, method Blessing 9 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585949, 4.831863 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.71 10 10 18.80 100.00 188 1.61 - 1.21 10 10 29.30 100.00 293 1.17 - 1.01 10 10 37.90 100.00 379 0.99 - 0.89 10 10 37.50 100.00 375 0.88 - 0.81 10 10 35.70 100.00 357 0.81 - 0.74 10 10 31.20 100.00 312 0.73 - 0.71 10 10 33.90 100.00 339 0.70 - 0.66 10 10 28.60 100.00 286 0.66 - 0.64 10 10 26.50 100.00 265 0.63 - 0.60 10 10 25.30 100.00 253 --------------------------------------------------------------- 8.38 - 0.60 100 100 30.47 100.00 3047 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:41:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362428 8.373725 8.370946 90.0239 90.0215 90.0252 3203 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.44 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1646 0 2148 2147 3203 N (int>3sigma) = 0 0 0 0 1646 0 2087 2081 3111 Mean intensity = 0.0 0.0 0.0 0.0 30.3 0.0 74.6 77.4 75.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 23.5 23.7 23.4 Lattice type: F chosen Volume: 586.17 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.97 90.06 119.93 Niggli form: a.a = 34.988 b.b = 34.997 c.c = 35.014 b.c = -17.489 a.c = -0.036 a.b = -17.461 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.082 CUBIC F-lattice R(int) = 0.044 [ 3046] Vol = 586.2 Cell: 8.362 8.374 8.371 89.98 89.98 90.03 Volume: 586.17 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.049 [ 2767] Vol = 439.6 Cell: 5.916 5.915 14.498 89.97 90.04 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.081 RHOMBOHEDRAL R-lattice R(int) = 0.041 [ 882] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.498 89.97 90.04 119.93 Volume: 439.63 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.058 TETRAGONAL I-lattice R(int) = 0.042 [ 2797] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.00 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.047 TETRAGONAL I-lattice R(int) = 0.042 [ 2797] Vol = 293.1 Cell: 5.921 5.919 8.362 89.97 90.00 90.02 Volume: 293.09 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.031 ORTHORHOMBIC I-lattice R(int) = 0.043 [ 2743] Vol = 293.1 Cell: 5.921 8.362 5.919 89.97 89.98 90.00 Volume: 293.09 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.011 MONOCLINIC I-lattice R(int) = 0.041 [ 2393] Vol = 293.1 Cell: 8.362 5.921 5.919 90.02 90.03 90.00 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.048 MONOCLINIC I-lattice R(int) = 0.040 [ 2397] Vol = 293.1 Cell: 5.917 5.915 8.374 89.97 90.00 89.94 Volume: 293.09 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.039 MONOCLINIC C-lattice R(int) = 0.041 [ 2408] Vol = 293.1 Cell: 8.362 8.374 5.915 89.97 134.96 90.03 Volume: 293.09 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.037 [ 1743] Vol = 146.5 Cell: 5.915 5.916 5.917 119.97 90.06 119.93 Volume: 146.54 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1646 0 2147 2148 3203 N (int>3sigma) = 0 0 0 0 1646 0 2081 2087 3111 Mean intensity = 0.0 0.0 0.0 0.0 30.3 0.0 77.4 74.6 75.3 Mean int/sigma = 0.0 0.0 0.0 0.0 24.2 0.0 23.7 23.5 23.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.176 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 31 31 232 722 N I>3s 31 31 220 722 0.9 0.9 0.7 36.0 8.5 8.5 5.3 27.0 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.044 2834 Fd-3m 1 1 227 C N N N N 37 2284 0.044 2873 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362428 8.373725 8.370946 89.9761 89.9785 90.0252 ZERR 3.00 0.000612 0.000700 0.000511 0.0058 0.0055 0.0063 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3901652- 505195 747 732 27 27.1 1148675.18 52.76 0.042 0.047 500903- 118690 923 920 27 34.1 200565.41 26.78 0.048 0.068 106895- 35059 797 797 27 29.5 78609.60 10.68 0.067 0.088 10102- 1826 758 754 29 26.0 3485.90 2.72 0.170 0.230 ------------------------------------------------------------------------------------------- 3901652- 1826 3225 3203 110 29.1 340502.85 23.05 0.045 0.053 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 812 793 27 29.4 591740.41 42.74 0.040 0.042 0.016 1.01-0.78 967 967 27 35.8 332334.88 21.03 0.038 0.047 0.029 0.78-0.65 833 830 28 29.6 250587.35 15.66 0.055 0.065 0.042 0.65-0.59 613 613 28 21.9 150122.59 10.76 0.075 0.094 0.059 ------------------------------------------------------------------------------------------------------ inf-0.59 3225 3203 110 29.1 340502.85 23.05 0.045 0.053 0.028 inf-0.60 3067 3045 99 30.8 352445.18 23.76 0.045 0.051 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 793 27 27 100.0 29.4 591740.41 236.07 0.040 0.003 1.01-0.78 967 27 27 100.0 35.8 332334.88 126.85 0.038 0.005 0.78-0.65 830 28 28 100.0 29.6 250587.35 90.04 0.055 0.009 0.65-0.59 613 28 28 100.0 21.9 150122.59 56.41 0.075 0.017 -------------------------------------------------------------------------------------------- inf-0.59 3203 110 110 100.0 29.1 340502.85 130.87 0.045 0.006 inf-0.60 3045 99 99 100.0 30.8 352445.18 135.40 0.045 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:46:46 2018) ID: 2932; threads 39; handles 878; mem 520424.00 (1237704.00)kB; time: 1w 5d 0h 52m 16s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.2,peak PF: 697.1, WS: 298.9, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:510.0,peak PF: 697.1, WS: 300.7, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:46:46 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00061 ) 8.37691 ( 0.00070 ) 8.37554 ( 0.00051 ) 90.02113 ( 0.00584 ) 90.03240 ( 0.00548 ) 90.03043 ( 0.00634 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:46:46 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007180 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(7) 8.3755(5) 90.021(6) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.3690(2) 8.3690(2) 8.3690(2) 90.0 90.0 90.0 V = 586.17(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 412 peaks identified as outliers and rejected 408 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 408 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 408 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.69 | 41 | 0.976 ( 0.056) | 0.930 ( 0.112) | 1.066 ( 0.427) | 0.69- 0.66 | 41 | 0.961 ( 0.041) | 0.913 ( 0.095) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.919 ( 0.025) | 0.850 ( 0.039) | 1.228 ( 0.480) | 0.63- 0.59 | 39 | 0.897 ( 0.037) | 0.833 ( 0.061) | 1.268 ( 0.459) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 408 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.125 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 408 obs out of 408 (total:408,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079342 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072164 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036321 -0.003695 0.076124 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3924(14) 8.4092(11) 89.968(12) 89.915(12) 90.079(14) V = 592.52(16) OTKP changes: 408 1 1 1 No constraint UB - matrix: -0.024797 -0.079513 -0.015578 ( 0.000012 0.000013 0.000010 ) 0.072430 -0.029115 0.032886 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003675 0.076437 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007183 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024797 -0.079513 -0.015578 ( 0.000012 0.000013 0.000010 ) 0.072430 -0.029115 0.032886 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003675 0.076437 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 408 obs out of 408 (total:408,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3688(13) 8.3785(10) 90.002(11) 89.975(11) 89.969(13) V = 587.13(15) unit cell: 8.3736(3) 8.3736(3) 8.3736(3) 90.0 90.0 90.0 V = 587.13(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024797 -0.079513 -0.015578 ( 0.000012 0.000013 0.000010 ) 0.072430 -0.029115 0.032886 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003675 0.076437 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007183 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024797 -0.079513 -0.015578 ( 0.000012 0.000013 0.000010 ) 0.072430 -0.029115 0.032886 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003675 0.076437 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 408 obs out of 408 (total:408,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3688(13) 8.3785(10) 90.002(11) 89.975(11) 89.969(13) V = 587.13(15) unit cell: 8.3736(3) 8.3736(3) 8.3736(3) 90.0 90.0 90.0 V = 587.13(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 408 obs out of 408 (total:408,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.099 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.025 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007215 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029290 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029290 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.55(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.55(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029290 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029290 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.55(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.55(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.046) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.985 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb PROFFITPEAK info: 626 peaks in the peak location table UB fit with 269 obs out of 303 (total:303,skipped:0) (88.78%) UB - matrix: -0.025124 -0.079486 -0.015643 ( 0.000050 0.000047 0.000028 ) 0.072566 -0.029443 0.032861 ( 0.000079 0.000075 0.000045 ) -0.036025 -0.003580 0.076527 ( 0.000038 0.000035 0.000021 ) M - matrix: 0.007195 -0.000011 0.000021 ( 0.000012 0.000007 0.000005 ) -0.000011 0.007198 0.000002 ( 0.000007 0.000009 0.000005 ) 0.000021 0.000002 0.007181 ( 0.000005 0.000005 0.000004 ) unit cell: 8.362(6) 8.360(5) 8.370(3) 90.02(4) 90.17(4) 89.92(6) V = 585.2(6) UB fit with 269 obs out of 303 (total:303,skipped:0) (88.78%) UB - matrix: -0.025124 -0.079486 -0.015643 ( 0.000050 0.000047 0.000028 ) 0.072566 -0.029443 0.032861 ( 0.000079 0.000075 0.000045 ) -0.036025 -0.003580 0.076527 ( 0.000038 0.000035 0.000021 ) M - matrix: 0.007195 -0.000011 0.000021 ( 0.000012 0.000007 0.000005 ) -0.000011 0.007198 0.000002 ( 0.000007 0.000009 0.000005 ) 0.000021 0.000002 0.007181 ( 0.000005 0.000005 0.000004 ) unit cell: 8.362(6) 8.360(5) 8.370(3) 90.02(4) 90.17(4) 89.92(6) V = 585.2(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB fit with 273 obs out of 303 (total:303,skipped:0) (90.10%) UB - matrix: -0.025154 -0.079500 -0.015669 ( 0.000053 0.000049 0.000030 ) 0.072583 -0.029475 0.032849 ( 0.000078 0.000072 0.000044 ) -0.036033 -0.003561 0.076537 ( 0.000037 0.000034 0.000021 ) M - matrix: 0.007199 -0.000011 0.000021 ( 0.000012 0.000007 0.000005 ) -0.000011 0.007202 0.000005 ( 0.000007 0.000009 0.000005 ) 0.000021 0.000005 0.007183 ( 0.000005 0.000005 0.000004 ) unit cell: 8.360(6) 8.358(5) 8.369(3) 90.04(4) 90.16(4) 89.91(6) V = 584.8(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 303 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025155 -0.079503 -0.015671 ( 0.000053 0.000049 0.000030 ) 0.072583 -0.029476 0.032849 ( 0.000078 0.000072 0.000044 ) -0.036033 -0.003560 0.076538 ( 0.000037 0.000034 0.000021 ) M - matrix: 0.007199 -0.000011 0.000021 ( 0.000012 0.000007 0.000005 ) -0.000011 0.007202 0.000005 ( 0.000007 0.000009 0.000005 ) 0.000021 0.000005 0.007183 ( 0.000005 0.000005 0.000004 ) Constraint UB - matrix: -0.025155 -0.079503 -0.015671 ( 0.000053 0.000049 0.000030 ) 0.072583 -0.029476 0.032849 ( 0.000078 0.000072 0.000044 ) -0.036033 -0.003560 0.076538 ( 0.000037 0.000034 0.000021 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000002 ) UB fit with 273 obs out of 303 (total:303,skipped:0) (90.10%) unit cell: 8.360(6) 8.358(5) 8.369(3) 90.04(4) 90.16(4) 89.91(6) V = 584.7(6) unit cell: 8.3622(10) 8.3622(10) 8.3622(10) 90.0 90.0 90.0 V = 584.74(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 271 obs out of 303 (total:303,skipped:0) (89.44%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb 2 of 217 peaks identified as outliers and rejected 215 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 215 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 215 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.13- 1.60 | 22 | 1.017 ( 0.202) | 1.174 ( 0.547) | 1.299 ( 1.189) | 1.47- 1.17 | 22 | 1.021 ( 0.128) | 1.202 ( 0.543) | 1.124 ( 0.560) | 1.17- 1.02 | 22 | 1.016 ( 0.074) | 1.081 ( 0.102) | 1.009 ( 0.403) | 1.02- 0.92 | 22 | 0.998 ( 0.082) | 1.044 ( 0.162) | 0.988 ( 0.408) | 0.92- 0.82 | 22 | 1.020 ( 0.073) | 1.037 ( 0.121) | 1.078 ( 0.382) | 0.82- 0.75 | 22 | 0.975 ( 0.072) | 0.960 ( 0.115) | 1.138 ( 0.435) | 0.75- 0.71 | 22 | 0.952 ( 0.052) | 0.868 ( 0.066) | 1.247 ( 0.561) | 0.71- 0.67 | 22 | 0.949 ( 0.048) | 0.865 ( 0.044) | 1.229 ( 0.451) | 0.67- 0.62 | 22 | 0.924 ( 0.047) | 0.828 ( 0.037) | 1.480 ( 0.493) | 0.62- 0.59 | 17 | 0.907 ( 0.058) | 0.805 ( 0.033) | 1.470 ( 0.504) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.13- 0.59 | 215 | 0.979 ( 0.104) | 0.991 ( 0.294) | 1.200 ( 0.607) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 214 obs out of 215 (total:215,skipped:0) (99.53%) UB - matrix: -0.025208 -0.079616 -0.015475 ( 0.000038 0.000034 0.000022 ) 0.072591 -0.029397 0.032831 ( 0.000038 0.000034 0.000023 ) -0.036109 -0.003561 0.076602 ( 0.000023 0.000021 0.000014 ) M - matrix: 0.007209 0.000002 0.000007 ( 0.000006 0.000004 0.000003 ) 0.000002 0.007216 -0.000006 ( 0.000004 0.000006 0.000003 ) 0.000007 -0.000006 0.007185 ( 0.000003 0.000003 0.000003 ) unit cell: 8.354(3) 8.350(3) 8.3678(19) 89.95(2) 90.06(2) 90.01(3) V = 583.7(4) OTKP changes: 214 1 1 1 No constraint UB - matrix: -0.025289 -0.079367 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072418 -0.029480 0.032834 ( 0.000038 0.000034 0.000022 ) -0.036087 -0.003522 0.076595 ( 0.000022 0.000020 0.000013 ) M - matrix: 0.007186 -0.000001 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000001 0.007181 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000010 0.000007 0.007191 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: -0.025289 -0.079367 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072418 -0.029480 0.032834 ( 0.000038 0.000034 0.000022 ) -0.036087 -0.003522 0.076595 ( 0.000022 0.000020 0.000013 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) UB fit with 214 obs out of 215 (total:215,skipped:0) (99.53%) unit cell: 8.367(3) 8.370(2) 8.3645(18) 90.06(2) 90.08(2) 89.99(3) V = 585.8(3) unit cell: 8.3674(5) 8.3674(5) 8.3674(5) 90.0 90.0 90.0 V = 585.83(6) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.853) HKL list info: 428 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025289 -0.079367 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072418 -0.029480 0.032834 ( 0.000038 0.000034 0.000022 ) -0.036087 -0.003522 0.076595 ( 0.000022 0.000020 0.000013 ) M - matrix: 0.007186 -0.000001 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000001 0.007181 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000010 0.000007 0.007191 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: -0.025289 -0.079367 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072418 -0.029480 0.032834 ( 0.000038 0.000034 0.000022 ) -0.036087 -0.003522 0.076595 ( 0.000022 0.000020 0.000013 ) M - matrix: 0.007178 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007178 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007178 ( 0.000000 0.000000 0.000001 ) UB fit with 214 obs out of 215 (total:215,skipped:0) (99.53%) unit cell: 8.367(3) 8.370(2) 8.3645(18) 90.06(2) 90.08(2) 89.99(3) V = 585.8(3) unit cell: 8.3674(5) 8.3674(5) 8.3674(5) 90.0 90.0 90.0 V = 585.83(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 214 obs out of 215 (total:215,skipped:0) (99.53%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb 2 of 218 peaks identified as outliers and rejected 216 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 216 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 216 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 1.61 | 22 | 1.015 ( 0.201) | 1.171 ( 0.541) | 1.294 ( 1.174) | 1.48- 1.17 | 22 | 1.040 ( 0.107) | 1.230 ( 0.508) | 1.122 ( 0.567) | 1.17- 1.04 | 22 | 0.987 ( 0.091) | 1.050 ( 0.142) | 1.017 ( 0.417) | 1.02- 0.92 | 22 | 1.024 ( 0.080) | 1.103 ( 0.150) | 0.927 ( 0.422) | 0.92- 0.84 | 22 | 0.993 ( 0.080) | 1.003 ( 0.133) | 1.061 ( 0.376) | 0.82- 0.75 | 22 | 0.976 ( 0.073) | 0.969 ( 0.119) | 1.113 ( 0.429) | 0.75- 0.71 | 22 | 0.961 ( 0.054) | 0.869 ( 0.067) | 1.289 ( 0.576) | 0.71- 0.67 | 22 | 0.944 ( 0.044) | 0.872 ( 0.046) | 1.180 ( 0.377) | 0.67- 0.62 | 22 | 0.928 ( 0.045) | 0.834 ( 0.037) | 1.414 ( 0.459) | 0.62- 0.59 | 18 | 0.906 ( 0.057) | 0.803 ( 0.033) | 1.530 ( 0.552) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.11- 0.59 | 216 | 0.979 ( 0.103) | 0.994 ( 0.289) | 1.188 ( 0.606) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 247 | 1.119 ( 0.135) | 1.241 ( 0.486) | 1.266 ( 1.142) | 13.0-18.8 | 247 | 1.078 ( 0.052) | 1.124 ( 0.228) | 1.166 ( 0.509) | 18.9-23.0 | 247 | 1.064 ( 0.069) | 1.143 ( 0.390) | 1.164 ( 0.555) | 23.0-27.2 | 247 | 1.031 ( 0.075) | 1.065 ( 0.244) | 1.153 ( 0.544) | 27.2-30.7 | 247 | 1.008 ( 0.074) | 1.007 ( 0.222) | 1.199 ( 0.496) | 30.7-33.8 | 247 | 0.976 ( 0.078) | 0.928 ( 0.111) | 1.203 ( 0.513) | 33.8-37.0 | 247 | 0.958 ( 0.074) | 0.900 ( 0.103) | 1.171 ( 0.480) | 37.0-39.7 | 247 | 0.940 ( 0.083) | 0.868 ( 0.128) | 1.226 ( 0.553) | 39.7-42.7 | 247 | 0.920 ( 0.077) | 0.837 ( 0.093) | 1.202 ( 0.548) | 42.8-49.9 | 244 | 0.924 ( 0.084) | 0.810 ( 0.063) | 1.156 ( 0.471) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2467 | 1.002 ( 0.106) | 0.993 ( 0.282) | 1.191 ( 0.612) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.26 e3 dimension: a=0.0019 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 23819788 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 15:47:17 2018 PROFFITMAIN - Started at Tue Mar 27 15:47:17 2018 OTKP changes: 2460 2 4 6 OTKP changes: 2460 2 4 6 No constraint UB - matrix: -0.025031 -0.079531 -0.015581 ( 0.000006 0.000007 0.000006 ) 0.072515 -0.029202 0.032942 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003596 0.076550 ( 0.000004 0.000005 0.000004 ) M - matrix: 0.007198 0.000003 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007191 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000002 0.007188 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025031 -0.079531 -0.015581 ( 0.000006 0.000007 0.000006 ) 0.072515 -0.029202 0.032942 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003596 0.076550 ( 0.000004 0.000005 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) UB fit with 2463 obs out of 2467 (total:2467,skipped:0) (99.84%) unit cell: 8.3605(5) 8.3645(6) 8.3662(5) 90.015(5) 90.042(5) 90.027(6) V = 585.06(7) unit cell: 8.36375(15) 8.36375(15) 8.36375(15) 90.0 90.0 90.0 V = 585.064(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033012 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024866 -0.079570 -0.015658 ( 0.000013 0.000015 0.000011 ) 0.072450 -0.029198 0.032949 ( 0.000016 0.000018 0.000013 ) -0.036286 -0.003652 0.076371 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000004 0.000005 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007197 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000005 0.000005 0.007163 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3685(15) 8.3607(15) 8.3805(10) 90.039(12) 90.043(12) 89.966(14) V = 586.36(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024983 -0.079528 -0.015506 ( 0.000017 0.000014 0.000012 ) 0.072503 -0.029258 0.033006 ( 0.000012 0.000010 0.000008 ) -0.036258 -0.003627 0.076509 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000006 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000010 0.007183 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3618(11) 8.3627(14) 8.3688(11) 89.920(12) 90.051(11) 89.977(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3570(14) 8.3624(11) 89.936(12) 90.002(11) 89.960(12) V = 583.94(15) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.94(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.759) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3570(14) 8.3624(11) 89.936(12) 90.002(11) 89.960(12) V = 583.94(15) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.94(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007194 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025021 -0.079578 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072547 -0.029299 0.032982 ( 0.000011 0.000010 0.000008 ) -0.036289 -0.003566 0.076597 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3570(14) 8.3624(11) 89.936(12) 90.002(11) 89.960(12) V = 583.94(15) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.94(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025016 -0.079537 -0.015716 ( 0.000008 0.000013 0.000012 ) 0.072414 -0.029341 0.032915 ( 0.000008 0.000014 0.000014 ) -0.036190 -0.003660 0.076522 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007179 -0.000003 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007200 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000004 0.007186 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3713(11) 8.3589(12) 8.3673(11) 90.033(11) 90.058(11) 89.980(11) V = 585.50(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3662(10) 8.3555(12) 8.3594(11) 89.995(11) 90.021(10) 90.029(11) V = 584.35(13) unit cell: 8.3604(3) 8.3604(3) 8.3604(3) 90.0 90.0 90.0 V = 584.35(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.759) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3662(10) 8.3555(12) 8.3594(11) 89.995(11) 90.021(10) 90.029(11) V = 584.35(13) unit cell: 8.3604(3) 8.3604(3) 8.3604(3) 90.0 90.0 90.0 V = 584.35(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007206 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079561 -0.015725 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029371 0.032984 ( 0.000008 0.000014 0.000013 ) -0.036298 -0.003694 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3662(10) 8.3555(12) 8.3594(11) 89.995(11) 90.021(10) 90.029(11) V = 584.35(13) unit cell: 8.3604(3) 8.3604(3) 8.3604(3) 90.0 90.0 90.0 V = 584.35(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025239 -0.079448 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072351 -0.029414 0.032794 ( 0.000008 0.000011 0.000012 ) -0.036263 -0.003615 0.076598 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007187 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007190 0.000011 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000011 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3670(10) 8.3649(14) 8.3641(11) 90.091(12) 89.944(10) 90.065(12) V = 585.39(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3598(10) 8.3607(14) 8.3565(11) 90.051(12) 89.994(10) 90.064(11) V = 584.06(14) unit cell: 8.3590(3) 8.3590(3) 8.3590(3) 90.0 90.0 90.0 V = 584.06(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.759) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3598(10) 8.3607(14) 8.3565(11) 90.051(12) 89.994(10) 90.064(11) V = 584.06(14) unit cell: 8.3590(3) 8.3590(3) 8.3590(3) 90.0 90.0 90.0 V = 584.06(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007197 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025255 -0.079489 -0.015749 ( 0.000011 0.000015 0.000017 ) 0.072464 -0.029419 0.032805 ( 0.000008 0.000011 0.000012 ) -0.036197 -0.003655 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3598(10) 8.3607(14) 8.3565(11) 90.051(12) 89.994(10) 90.064(11) V = 584.06(14) unit cell: 8.3590(3) 8.3590(3) 8.3590(3) 90.0 90.0 90.0 V = 584.06(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) UB - matrix: -0.025268 -0.079440 -0.015616 ( 0.000028 0.000025 0.000016 ) 0.072478 -0.029459 0.032841 ( 0.000038 0.000033 0.000022 ) -0.036110 -0.003522 0.076589 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007195 -0.000001 0.000009 ( 0.000006 0.000004 0.000003 ) -0.000001 0.007191 0.000003 ( 0.000004 0.000004 0.000002 ) 0.000009 0.000003 0.007188 ( 0.000003 0.000002 0.000003 ) unit cell: 8.362(3) 8.364(3) 8.3660(19) 90.03(2) 90.07(2) 89.99(3) V = 585.1(3) OTKP changes: 215 1 1 1 No constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007187 -0.000002 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000002 0.007179 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000010 0.000007 0.007190 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) unit cell: 8.367(3) 8.371(2) 8.3652(19) 90.06(2) 90.08(2) 89.99(3) V = 585.9(3) unit cell: 8.3677(5) 8.3677(5) 8.3677(5) 90.0 90.0 90.0 V = 585.89(6) Run 6 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.864) HKL list info: 421 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007187 -0.000002 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000002 0.007179 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000010 0.000007 0.007190 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) unit cell: 8.367(3) 8.371(2) 8.3652(19) 90.06(2) 90.08(2) 89.99(3) V = 585.9(3) unit cell: 8.3677(5) 8.3677(5) 8.3677(5) 90.0 90.0 90.0 V = 585.89(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007187 -0.000002 0.000010 ( 0.000006 0.000003 0.000003 ) -0.000002 0.007179 0.000007 ( 0.000003 0.000004 0.000002 ) 0.000010 0.000007 0.007190 ( 0.000003 0.000002 0.000003 ) Constraint UB - matrix: -0.025294 -0.079355 -0.015685 ( 0.000026 0.000023 0.000015 ) 0.072416 -0.029494 0.032836 ( 0.000038 0.000033 0.000022 ) -0.036102 -0.003515 0.076586 ( 0.000023 0.000020 0.000013 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) unit cell: 8.367(3) 8.371(2) 8.3652(19) 90.06(2) 90.08(2) 89.99(3) V = 585.9(3) unit cell: 8.3677(5) 8.3677(5) 8.3677(5) 90.0 90.0 90.0 V = 585.89(6) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025014 -0.079450 -0.015557 ( 0.000006 0.000007 0.000007 ) 0.072502 -0.029170 0.032907 ( 0.000006 0.000007 0.000007 ) -0.036224 -0.003573 0.076527 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007176 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007181 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025014 -0.079450 -0.015557 ( 0.000006 0.000007 0.000007 ) 0.072502 -0.029170 0.032907 ( 0.000006 0.000007 0.000007 ) -0.036224 -0.003573 0.076527 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2463 obs out of 2467 (total:2467,skipped:0) (99.84%) unit cell: 8.3624(6) 8.3731(7) 8.3701(5) 90.021(6) 90.023(5) 90.015(6) V = 586.07(7) unit cell: 8.3686(2) 8.3686(2) 8.3686(2) 90.0 90.0 90.0 V = 586.07(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 71 reflections under beam stop or inside a detector rejection region 21 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3338 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:47:25 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.759) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.759) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.759) Run 6 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.864) PROFFIT INFO: signal sum: min=255.0000 max=22921440.0000 PROFFIT INFO: signal sum lp corr: min=469.0958 max=2958241.0911 PROFFIT INFO: background sum: min=612.0000 max=26108.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=11938.0000 PROFFIT INFO: num of signal pixels: min=51 max=460 PROFFIT INFO: Inet: min=750.5533 max=4733185.5000 PROFFIT INFO: sig(Inet): min=120.2327 max=47790.2578 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.87 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 38 160 350 676 762 1373 2227 3062 3338 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.1 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3338 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3338 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4733186- 1124857 333 1862334.01 122.22 100.00 1123428- 621211 333 848564.51 102.38 100.00 620887- 265948 333 414358.11 94.98 100.00 265692- 169741 333 203330.95 71.93 100.00 169692- 120462 333 144793.69 51.04 100.00 120451- 93269 333 105712.50 36.08 100.00 93201- 65898 333 80455.83 29.24 100.00 65755- 5657 333 37916.38 19.32 100.00 5630- 2977 333 3963.69 5.29 97.00 2967- 751 341 2129.30 3.73 56.01 ------------------------------------------------------------------------------------ 4733186- 751 3338 369473.39 53.50 95.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 739273.59 93.96 100.00 1.41- 1.12 333 617174.49 63.90 99.40 1.12- 0.96 333 499734.28 70.68 97.90 0.96- 0.88 333 349940.98 59.74 94.59 0.88- 0.81 333 452039.45 68.92 99.70 0.81- 0.73 333 248270.09 41.62 95.20 0.73- 0.71 333 174959.02 34.12 88.59 0.71- 0.65 333 313830.38 47.68 93.99 0.65- 0.62 333 153938.34 27.37 87.99 0.62- 0.58 341 150826.07 27.64 94.72 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 369473.39 53.50 95.21 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:47:25 2018 Sorting 3338 observations 119 unique observations with > 7.00 F2/sig(F2) 3338 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 49 571 Total number of frames 571 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 5 frame = 1 scale 3338 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 9 116 Total number of frames 116 2683 observations > 7.00 F2/sig(F2) 2683 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 9 116 Total number of frames 116 Removing 'redundancy=1' reflections Average redundancy: 20.9 (Out of 2683 removed 5 = 2678, unique = 128) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2678 observations in 6 runs Run # start # end # total # 1 0 21 22 2 0 19 42 3 0 21 64 4 0 21 86 5 0 19 106 6 0 9 116 Total number of frames 116 128 unique data precomputed (should be 128) 128 unique data with 2678 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 20.9 (Out of 2678 removed 0 = 2678, unique = 128) 128 unique data precomputed (should be 128) 128 unique data with 2678 observations RMS deviation of equivalent data = 0.25779 Rint = 0.18884 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18133, wR= 0.26516 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13564, wR= 0.17301, Acormin=0.607, Acormax=1.415, Acor_av=0.987 F test: Probability=1.000, F= 1.784 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12091, wR= 0.15058, Acormin=0.559, Acormax=1.443, Acor_av=0.912 F test: Probability=1.000, F= 1.257 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10734, wR= 0.14223, Acormin=0.629, Acormax=1.563, Acor_av=0.970 F test: Probability=1.000, F= 1.266 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09166, wR= 0.12190, Acormin=0.536, Acormax=1.549, Acor_av=0.894 F test: Probability=1.000, F= 1.370 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07883, wR= 0.10966, Acormin=0.526, Acormax=1.615, Acor_av=0.911 F test: Probability=1.000, F= 1.348 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09861, wR= 0.13515, Acormin=0.632, Acormax=1.646, Acor_av=0.973 F test: Probability=0.000, F= 0.638 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08537, wR= 0.11649, Acormin=0.514, Acormax=1.617, Acor_av=0.900 F test: Probability=0.000, F= 0.851 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07526, wR= 0.10619, Acormin=0.509, Acormax=1.649, Acor_av=0.918 F test: Probability=0.986, F= 1.091 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07229, wR= 0.10045, Acormin=0.399, Acormax=1.531, Acor_av=0.868 F test: Probability=0.972, F= 1.079 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09936, wR= 0.12999, Acormin=0.460, Acormax=1.462, Acor_av=0.843 F test: Probability=0.000, F= 0.530 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08369, wR= 0.11158, Acormin=0.501, Acormax=1.592, Acor_av=0.888 F test: Probability=0.000, F= 0.746 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08328, wR= 0.11032, Acormin=0.114, Acormax=0.410, Acor_av=0.222 F test: Probability=0.000, F= 0.752 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07356, wR= 0.10041, Acormin=0.117, Acormax=0.438, Acor_av=0.250 F test: Probability=0.000, F= 0.959 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06788, wR= 0.09335, Acormin=0.129, Acormax=0.478, Acor_av=0.262 F test: Probability=0.998, F= 1.120 Final absorption model (ne=6, no=5): Rint= 0.07229, Acormin=0.399, Acormax=1.531, Acor_av=0.868 Combined refinement in use Rint: 0.18894 There are 116 active scales (one needs to be fixed) Refinement control: frame scale #115 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25779 Using Levenberg-Marquardt: 0.00010 New wR= 0.06139 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18884 with corrections 0.04866 Rint for all data: 0.18894 with corrections 0.04889 1 observations identified as outliers and rejected Cycle 2 wR= 0.06137 Using Levenberg-Marquardt: 0.00001 New wR= 0.05862 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18734 with corrections 0.04611 Rint for all data: 0.18894 with corrections 0.04644 0 observations identified as outliers and rejected Cycle 3 wR= 0.05862 Using Levenberg-Marquardt: 0.00000 New wR= 0.05800 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18734 with corrections 0.04565 Rint for all data: 0.18894 with corrections 0.04598 0 observations identified as outliers and rejected Cycle 4 wR= 0.05800 Using Levenberg-Marquardt: 0.00000 New wR= 0.05764 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18734 with corrections 0.04537 Rint for all data: 0.18894 with corrections 0.04570 0 observations identified as outliers and rejected Cycle 5 wR= 0.05764 Using Levenberg-Marquardt: 0.00000 New wR= 0.05742 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18734 with corrections 0.04520 Rint for all data: 0.18894 with corrections 0.04552 0 observations identified as outliers and rejected Final wR= 0.05742 Final frame scales: Min= 0.7385 Max= 1.2988 Final absorption correction factors: Amin= 0.5073 Amax= 1.4314 PROFFIT INFO: Inet (after scale3 abspack): min=762.4594 max=4583176.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=145.0268 max=52993.1094 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3338 reflections read from tmp file 702 reflections are rejected (701 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 6 5 2 3 1 5 6 10 117 Initial Chi^2= 0.42866 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.97966 Current error model SIG(F2)^2 = 161.24*I_RAW + 0.00*I_BACK+(0.01413*)^2 Cycle 2, Chi^2= 1.02389 Current error model SIG(F2)^2 = 104.11*I_RAW + 0.00*I_BACK+(0.02272*)^2 Cycle 3, Chi^2= 1.00089 Current error model SIG(F2)^2 = 117.51*I_RAW + 0.00*I_BACK+(0.02041*)^2 Cycle 4, Chi^2= 0.99996 Current error model SIG(F2)^2 = 116.37*I_RAW + 0.00*I_BACK+(0.02069*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 116.56*I_RAW + 0.00*I_BACK+(0.02065*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 116.56*I_RAW + 0.00*I_BACK+(0.02065*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4583176- 1089282 333 1752680.87 45.00 100.00 1088831- 605232 333 808541.88 37.77 100.00 604515- 257234 333 402387.06 36.33 100.00 257155- 153420 333 192122.27 31.72 100.00 153392- 124123 333 138995.99 25.77 100.00 124045- 87459 333 102189.35 19.70 100.00 87432- 68050 333 78406.05 16.95 100.00 68005- 5051 333 40064.49 12.17 100.00 4975- 2737 333 3638.26 4.62 96.40 2732- 762 341 2141.24 3.78 75.07 ------------------------------------------------------------------------------------ 4583176- 762 3338 351277.98 23.33 97.09 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 738535.20 36.82 100.00 1.41- 1.12 333 596707.34 28.99 99.40 1.12- 0.96 333 457937.04 27.94 98.80 0.96- 0.88 333 329090.69 23.86 97.00 0.88- 0.81 333 426410.53 27.39 99.70 0.81- 0.73 333 227884.09 19.12 96.40 0.73- 0.71 333 165472.59 17.39 92.19 0.71- 0.65 333 293711.14 22.47 97.90 0.65- 0.62 333 143280.09 14.56 92.49 0.62- 0.58 341 138854.35 15.01 97.07 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 351277.98 23.33 97.09 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 738535.20 36.82 100.00 4.82- 1.12 666 667621.27 32.91 99.70 4.82- 0.96 999 597726.53 31.25 99.40 4.82- 0.88 1332 530567.57 29.40 98.80 4.82- 0.81 1665 509736.16 29.00 98.98 4.82- 0.73 1998 462760.81 27.35 98.55 4.82- 0.71 2331 420291.07 25.93 97.64 4.82- 0.65 2664 404468.58 25.50 97.67 4.82- 0.62 2997 375447.63 24.28 97.10 4.82- 0.58 3338 351277.98 23.33 97.09 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 351277.98 23.33 97.09 Scale applied to data: s=0.218189 (maximum obs:4583176.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.046; Rsigma 0.028: data 3338 -> merged 157 With outlier rejection... Rint 0.045; Rsigma 0.028: data 3325 -> merged 157 Rejected total: 13, method kkm 12, method Blessing 1 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585917, 4.831592 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 19.21 100.00 269 1.41 - 1.12 14 14 27.29 100.00 382 1.12 - 0.97 14 14 27.29 100.00 382 0.96 - 0.84 14 14 29.21 100.00 409 0.84 - 0.78 14 14 22.50 100.00 315 0.78 - 0.73 14 14 23.29 100.00 326 0.73 - 0.69 14 14 21.93 100.00 307 0.69 - 0.66 14 14 18.86 100.00 264 0.65 - 0.63 14 14 19.29 100.00 270 0.63 - 0.60 14 14 17.21 100.00 241 --------------------------------------------------------------- 8.37 - 0.60 140 140 22.61 100.00 3165 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:47:26 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362442 8.373141 8.370109 90.0214 90.0227 90.0154 3325 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1706 0 2233 2232 3325 N (int>3sigma) = 0 0 0 0 1706 0 2168 2160 3228 Mean intensity = 0.0 0.0 0.0 0.0 30.6 0.0 76.6 79.0 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.07 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.98 90.05 119.94 Niggli form: a.a = 34.983 b.b = 35.001 c.c = 35.011 b.c = -17.491 a.c = -0.032 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.045 [ 3168] Vol = 586.1 Cell: 8.362 8.373 8.370 89.98 89.98 90.02 Volume: 586.07 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 2888] Vol = 439.6 Cell: 5.916 5.915 14.496 89.97 90.04 119.94 Volume: 439.56 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.040 [ 919] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.496 89.97 90.04 119.94 Volume: 439.56 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.047 TETRAGONAL I-lattice R(int) = 0.044 [ 2919] Vol = 293.0 Cell: 5.921 5.919 8.362 89.97 89.99 90.02 Volume: 293.04 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.044 TETRAGONAL I-lattice R(int) = 0.044 [ 2919] Vol = 293.0 Cell: 5.921 5.919 8.362 89.97 89.99 90.02 Volume: 293.04 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 2864] Vol = 293.0 Cell: 5.921 8.362 5.919 89.97 89.98 90.01 Volume: 293.04 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.043 [ 2514] Vol = 293.0 Cell: 8.362 5.921 5.919 90.02 90.03 90.01 Volume: 293.04 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.026 MONOCLINIC C-lattice R(int) = 0.042 [ 2529] Vol = 293.0 Cell: 8.362 8.373 5.915 89.97 134.96 90.02 Volume: 293.04 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.039 [ 1860] Vol = 146.5 Cell: 5.915 5.916 5.917 119.98 90.05 119.94 Volume: 146.52 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1706 0 2232 2233 3325 N (int>3sigma) = 0 0 0 0 1706 0 2160 2168 3228 Mean intensity = 0.0 0.0 0.0 0.0 30.6 0.0 79.0 76.6 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.5 23.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 242 743 N I>3s 34 34 230 743 1.0 1.0 0.7 36.4 8.8 8.8 5.3 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.045 2946 Fd-3m 1 1 227 C N N N N 37 2284 0.046 2985 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362442 8.373141 8.370109 89.9786 89.9773 90.0154 ZERR 3.00 0.000609 0.000678 0.000500 0.0057 0.0054 0.0062 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3921685- 743945 548 547 26 21.0 1411486.06 42.60 0.039 0.055 739048- 221948 516 514 26 19.8 442859.84 36.40 0.060 0.076 218952- 96727 776 776 26 29.8 147305.43 26.32 0.041 0.053 94272- 69783 532 530 26 20.4 81825.07 17.07 0.068 0.086 64864- 3600 436 433 26 16.7 26038.93 9.12 0.084 0.110 3384- 1714 530 525 27 19.4 2618.07 4.17 0.186 0.240 ------------------------------------------------------------------------------------------- 3921685- 1714 3338 3325 157 21.2 351891.27 23.34 0.045 0.061 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 621 614 26 23.6 609928.29 32.20 0.046 0.063 0.023 1.12-0.88 735 734 26 28.2 457723.41 27.18 0.033 0.045 0.025 0.85-0.75 621 621 26 23.9 326031.07 22.79 0.040 0.051 0.029 0.74-0.68 542 540 26 20.8 254747.50 20.38 0.056 0.065 0.033 0.67-0.63 512 511 26 19.7 147043.76 16.07 0.073 0.091 0.042 0.62-0.59 307 305 27 11.3 145590.86 14.86 0.075 0.083 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3338 3325 157 21.2 351891.27 23.34 0.045 0.061 0.028 inf-0.60 3175 3163 139 22.8 364500.38 23.84 0.045 0.060 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 614 26 26 100.0 23.6 609928.29 170.75 0.046 0.006 1.12-0.88 734 26 26 100.0 28.2 457723.41 147.00 0.033 0.005 0.85-0.75 621 26 26 100.0 23.9 326031.07 118.35 0.040 0.006 0.74-0.68 540 26 26 100.0 20.8 254747.50 95.17 0.056 0.008 0.67-0.63 511 26 26 100.0 19.7 147043.76 70.74 0.073 0.010 0.62-0.59 305 27 27 100.0 11.3 145590.86 58.22 0.075 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3325 157 157 100.0 21.2 351891.27 117.75 0.045 0.007 inf-0.60 3163 139 139 100.0 22.8 364500.38 121.32 0.045 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025014 -0.079450 -0.015557 ( 0.000006 0.000007 0.000007 ) 0.072502 -0.029170 0.032907 ( 0.000006 0.000007 0.000007 ) -0.036224 -0.003573 0.076527 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007176 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007181 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025014 -0.079450 -0.015557 ( 0.000006 0.000007 0.000007 ) 0.072502 -0.029170 0.032907 ( 0.000006 0.000007 0.000007 ) -0.036224 -0.003573 0.076527 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3624(6) 8.3731(7) 8.3701(5) 90.021(6) 90.023(5) 90.015(6) V = 586.07(7) unit cell: 8.3686(2) 8.3686(2) 8.3686(2) 90.0 90.0 90.0 V = 586.07(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.759) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.759) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.759) Run 6 Omega scan: (-1.000 - 49.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.864) PROFFIT INFO: signal sum: min=255.0000 max=22921440.0000 PROFFIT INFO: signal sum lp corr: min=469.0958 max=2958241.0911 PROFFIT INFO: background sum: min=612.0000 max=26108.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=11938.0000 PROFFIT INFO: num of signal pixels: min=51 max=460 PROFFIT INFO: Inet: min=750.5533 max=4733185.5000 PROFFIT INFO: sig(Inet): min=120.2327 max=47790.2578 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.87 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 76 320 700 1352 1524 2746 4454 6124 6676 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.1 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3338 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3338 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4733186- 1124857 333 1862334.01 122.22 100.00 1123428- 621211 333 848564.51 102.38 100.00 620887- 265948 333 414358.11 94.98 100.00 265692- 169741 333 203330.95 71.93 100.00 169692- 120462 333 144793.69 51.04 100.00 120451- 93269 333 105712.50 36.08 100.00 93201- 65898 333 80455.83 29.24 100.00 65755- 5657 333 37916.38 19.32 100.00 5630- 2977 333 3963.69 5.29 97.00 2967- 751 341 2129.30 3.73 56.01 ------------------------------------------------------------------------------------ 4733186- 751 3338 369473.39 53.50 95.21 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 739273.59 93.96 100.00 1.41- 1.12 333 617174.49 63.90 99.40 1.12- 0.96 333 499734.28 70.68 97.90 0.96- 0.88 333 349940.98 59.74 94.59 0.88- 0.81 333 452039.45 68.92 99.70 0.81- 0.73 333 248270.09 41.62 95.20 0.73- 0.71 333 174959.02 34.12 88.59 0.71- 0.65 333 313830.38 47.68 93.99 0.65- 0.62 333 153938.34 27.37 87.99 0.62- 0.58 341 150826.07 27.64 94.72 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 369473.39 53.50 95.21 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:47:27 2018 Sorting 3338 observations 86 unique observations with > 7.00 F2/sig(F2) 3338 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 49 571 Total number of frames 571 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3338 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 7 86 Total number of frames 86 2683 observations > 7.00 F2/sig(F2) 2683 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 7 86 Total number of frames 86 Removing 'redundancy=1' reflections Average redundancy: 28.8 (Out of 2683 removed 3 = 2680, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2680 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 7 86 Total number of frames 86 93 unique data precomputed (should be 93) 93 unique data with 2680 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 28.8 (Out of 2680 removed 0 = 2680, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2680 observations RMS deviation of equivalent data = 0.25814 Rint = 0.18905 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18146, wR= 0.26555 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13585, wR= 0.17355, Acormin=0.606, Acormax=1.415, Acor_av=0.987 F test: Probability=1.000, F= 1.781 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12133, wR= 0.15116, Acormin=0.559, Acormax=1.443, Acor_av=0.911 F test: Probability=1.000, F= 1.252 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10768, wR= 0.14275, Acormin=0.628, Acormax=1.563, Acor_av=0.971 F test: Probability=1.000, F= 1.267 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09175, wR= 0.12247, Acormin=0.534, Acormax=1.547, Acor_av=0.894 F test: Probability=1.000, F= 1.376 Trying model 5 (ne=4, no=3)... Results: Rint= 0.07895, wR= 0.11027, Acormin=0.523, Acormax=1.613, Acor_av=0.911 F test: Probability=1.000, F= 1.347 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09849, wR= 0.13543, Acormin=0.633, Acormax=1.652, Acor_av=0.975 F test: Probability=0.000, F= 0.642 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08531, wR= 0.11680, Acormin=0.517, Acormax=1.617, Acor_av=0.902 F test: Probability=0.000, F= 0.854 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07524, wR= 0.10653, Acormin=0.511, Acormax=1.654, Acor_av=0.918 F test: Probability=0.989, F= 1.096 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07234, wR= 0.10085, Acormin=0.404, Acormax=1.532, Acor_av=0.869 F test: Probability=0.969, F= 1.077 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09934, wR= 0.13065, Acormin=0.473, Acormax=1.458, Acor_av=0.846 F test: Probability=0.000, F= 0.531 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08347, wR= 0.11194, Acormin=0.504, Acormax=1.603, Acor_av=0.890 F test: Probability=0.000, F= 0.751 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08337, wR= 0.11112, Acormin=0.113, Acormax=0.408, Acor_av=0.220 F test: Probability=0.000, F= 0.751 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07396, wR= 0.10130, Acormin=0.118, Acormax=0.434, Acor_av=0.247 F test: Probability=0.000, F= 0.950 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06792, wR= 0.09401, Acormin=0.128, Acormax=0.472, Acor_av=0.258 F test: Probability=0.998, F= 1.120 Final absorption model (ne=6, no=5): Rint= 0.07234, Acormin=0.404, Acormax=1.532, Acor_av=0.869 Combined refinement in use Rint: 0.18915 There are 86 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 133 pars with 8911 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25814 Using Levenberg-Marquardt: 0.00010 New wR= 0.06364 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18905 with corrections 0.05080 Rint for all data: 0.18915 with corrections 0.05102 1 observations identified as outliers and rejected Cycle 2 wR= 0.06362 Using Levenberg-Marquardt: 0.00001 New wR= 0.06075 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18755 with corrections 0.04806 Rint for all data: 0.18915 with corrections 0.04837 0 observations identified as outliers and rejected Cycle 3 wR= 0.06075 Using Levenberg-Marquardt: 0.00000 New wR= 0.06003 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18755 with corrections 0.04754 Rint for all data: 0.18915 with corrections 0.04785 0 observations identified as outliers and rejected Cycle 4 wR= 0.06003 Using Levenberg-Marquardt: 0.00000 New wR= 0.05962 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18755 with corrections 0.04725 Rint for all data: 0.18915 with corrections 0.04756 0 observations identified as outliers and rejected Cycle 5 wR= 0.05962 Using Levenberg-Marquardt: 0.00000 New wR= 0.05933 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18755 with corrections 0.04706 Rint for all data: 0.18915 with corrections 0.04738 0 observations identified as outliers and rejected Final wR= 0.05933 Final frame scales: Min= 0.7561 Max= 1.2606 Final absorption correction factors: Amin= 0.4970 Amax= 1.4435 PROFFIT INFO: Inet (after scale3 abspack): min=774.6908 max=4587123.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=146.0395 max=53094.5039 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3338 reflections read from tmp file 740 reflections are rejected (740 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 2 1 1 3 4 6 85 Initial Chi^2= 0.40125 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.27859 Current error model SIG(F2)^2 = 161.72*I_RAW + 0.00*I_BACK+(0.00915*)^2 Cycle 2, Chi^2= 1.21013 Current error model SIG(F2)^2 = 67.49*I_RAW + 0.00*I_BACK+(0.02581*)^2 Cycle 3, Chi^2= 1.00229 Current error model SIG(F2)^2 = 112.67*I_RAW + 0.00*I_BACK+(0.02022*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 110.19*I_RAW + 0.00*I_BACK+(0.02079*)^2 Cycle 5, Chi^2= 1.00003 Current error model SIG(F2)^2 = 110.84*I_RAW + 0.00*I_BACK+(0.02066*)^2 Cycle 6, Chi^2= 0.99999 Current error model SIG(F2)^2 = 110.69*I_RAW + 0.00*I_BACK+(0.02069*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 110.69*I_RAW + 0.00*I_BACK+(0.02069*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4587124- 1090198 333 1750489.66 45.15 100.00 1082517- 604106 333 809924.44 38.13 100.00 603780- 256043 333 402504.19 36.70 100.00 254245- 153641 333 191936.56 32.14 100.00 153576- 123829 333 138857.06 26.15 100.00 123773- 87394 333 102234.95 20.11 100.00 87375- 68405 333 78522.77 17.35 100.00 68296- 5024 333 40128.88 12.44 100.00 5019- 2744 333 3643.06 4.75 98.20 2735- 775 341 2142.36 3.87 78.01 ------------------------------------------------------------------------------------ 4587124- 775 3338 351199.82 23.63 97.57 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 737108.69 37.02 100.00 1.41- 1.12 333 595830.28 29.27 99.40 1.12- 0.96 333 457249.64 28.22 98.80 0.96- 0.88 333 329091.52 24.17 97.90 0.88- 0.81 333 426841.83 27.73 99.70 0.81- 0.73 333 228126.76 19.42 97.30 0.73- 0.71 333 165501.79 17.71 93.39 0.71- 0.65 333 294226.48 22.83 97.90 0.65- 0.62 333 143956.23 14.84 93.39 0.62- 0.58 341 139159.01 15.30 97.95 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 351199.82 23.63 97.57 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 333 737108.69 37.02 100.00 4.82- 1.12 666 666469.48 33.15 99.70 4.82- 0.96 999 596729.53 31.51 99.40 4.82- 0.88 1332 529820.03 29.67 99.02 4.82- 0.81 1665 509224.39 29.28 99.16 4.82- 0.73 1998 462374.79 27.64 98.85 4.82- 0.71 2331 419964.36 26.22 98.07 4.82- 0.65 2664 404247.12 25.80 98.05 4.82- 0.62 2997 375325.91 24.58 97.53 4.82- 0.58 3338 351199.82 23.63 97.57 ------------------------------------------------------------------------------------ 4.82- 0.58 3338 351199.82 23.63 97.57 Scale applied to data: s=0.218001 (maximum obs:4587123.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.027: data 3338 -> merged 110 With outlier rejection... Rint 0.047; Rsigma 0.027: data 3330 -> merged 110 Rejected total: 8, method kkm 7, method Blessing 1 Completeness direct cell (a, b, c) = (8.369, 8.369, 8.369), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585917, 4.831593 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 20.60 100.00 206 1.61 - 1.21 10 10 30.40 100.00 304 1.17 - 1.01 10 10 39.40 100.00 394 0.99 - 0.89 10 10 38.90 100.00 389 0.88 - 0.81 10 10 37.20 100.00 372 0.81 - 0.74 10 10 32.00 100.00 320 0.73 - 0.71 10 10 35.20 100.00 352 0.70 - 0.66 10 10 29.90 100.00 299 0.66 - 0.64 10 10 27.10 100.00 271 0.63 - 0.60 10 10 26.20 100.00 262 --------------------------------------------------------------- 8.37 - 0.60 100 100 31.69 100.00 3169 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:47:26 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.362442 8.373141 8.370109 90.0214 90.0227 90.0154 3325 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.34 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1706 0 2233 2232 3325 N (int>3sigma) = 0 0 0 0 1706 0 2168 2160 3228 Mean intensity = 0.0 0.0 0.0 0.0 30.6 0.0 76.6 79.0 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.07 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.915 5.916 5.917 119.98 90.05 119.94 Niggli form: a.a = 34.983 b.b = 35.001 c.c = 35.011 b.c = -17.491 a.c = -0.032 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.071 CUBIC F-lattice R(int) = 0.045 [ 3168] Vol = 586.1 Cell: 8.362 8.373 8.370 89.98 89.98 90.02 Volume: 586.07 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 2888] Vol = 439.6 Cell: 5.916 5.915 14.496 89.97 90.04 119.94 Volume: 439.56 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.070 RHOMBOHEDRAL R-lattice R(int) = 0.040 [ 919] Vol = 439.6 Trigonal Cell: 5.916 5.915 14.496 89.97 90.04 119.94 Volume: 439.56 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.047 TETRAGONAL I-lattice R(int) = 0.044 [ 2919] Vol = 293.0 Cell: 5.921 5.919 8.362 89.97 89.99 90.02 Volume: 293.04 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.044 TETRAGONAL I-lattice R(int) = 0.044 [ 2919] Vol = 293.0 Cell: 5.921 5.919 8.362 89.97 89.99 90.02 Volume: 293.04 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.035 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 2864] Vol = 293.0 Cell: 5.921 8.362 5.919 89.97 89.98 90.01 Volume: 293.04 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.018 MONOCLINIC I-lattice R(int) = 0.043 [ 2514] Vol = 293.0 Cell: 8.362 5.921 5.919 90.02 90.03 90.01 Volume: 293.04 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.026 MONOCLINIC C-lattice R(int) = 0.042 [ 2529] Vol = 293.0 Cell: 8.362 8.373 5.915 89.97 134.96 90.02 Volume: 293.04 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.039 [ 1860] Vol = 146.5 Cell: 5.915 5.916 5.917 119.98 90.05 119.94 Volume: 146.52 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1706 0 2232 2233 3325 N (int>3sigma) = 0 0 0 0 1706 0 2160 2168 3228 Mean intensity = 0.0 0.0 0.0 0.0 30.6 0.0 79.0 76.6 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.5 23.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 34 34 242 743 N I>3s 34 34 230 743 1.0 1.0 0.7 36.4 8.8 8.8 5.3 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.045 2946 Fd-3m 1 1 227 C N N N N 37 2284 0.046 2985 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362442 8.373141 8.370109 89.9786 89.9773 90.0154 ZERR 3.00 0.000609 0.000678 0.000500 0.0057 0.0054 0.0062 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3930033- 505484 739 739 27 27.4 1209153.78 40.78 0.045 0.061 502054- 118606 996 996 27 36.9 212361.35 31.00 0.051 0.071 106323- 35108 822 820 27 30.4 78320.38 17.22 0.067 0.086 10006- 1849 781 775 29 26.7 3476.01 4.67 0.165 0.218 ------------------------------------------------------------------------------------------- 3930033- 1849 3338 3330 110 30.3 351949.90 23.65 0.047 0.064 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 842 837 27 31.0 628872.30 33.21 0.044 0.064 0.023 1.01-0.78 1026 1025 28 36.6 325583.09 22.90 0.037 0.047 0.028 0.76-0.65 882 882 28 31.5 246106.16 20.04 0.057 0.071 0.033 0.65-0.59 588 586 27 21.7 161840.87 16.72 0.077 0.092 0.040 ------------------------------------------------------------------------------------------------------ inf-0.59 3338 3330 110 30.3 351949.90 23.65 0.047 0.064 0.027 inf-0.60 3175 3167 99 32.0 364485.70 24.14 0.047 0.063 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 837 27 27 100.0 31.0 628872.30 208.01 0.044 0.006 1.01-0.78 1025 28 28 100.0 36.6 325583.09 148.74 0.037 0.005 0.76-0.65 882 28 28 100.0 31.5 246106.16 120.01 0.057 0.007 0.65-0.59 586 27 27 100.0 21.7 161840.87 90.13 0.077 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3330 110 110 100.0 30.3 351949.90 145.71 0.047 0.006 inf-0.60 3167 99 99 100.0 32.0 364485.70 149.66 0.047 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 15:54:12 2018) ID: 2932; threads 39; handles 878; mem 516564.00 (1237704.00)kB; time: 1w 5d 0h 59m 43s MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:504.5,peak PF: 697.1, WS: 295.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.2,peak PF: 697.1, WS: 297.1, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 15:54:12 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00061 ) 8.37691 ( 0.00068 ) 8.37554 ( 0.00050 ) 90.02113 ( 0.00569 ) 90.03240 ( 0.00542 ) 90.03043 ( 0.00623 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 15:54:12 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007194 0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007176 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007181 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(7) 8.3755(5) 90.021(6) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.3686(2) 8.3686(2) 8.3686(2) 90.0 90.0 90.0 V = 586.07(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 448 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.982 ( 0.167) | 1.293 ( 0.709) | 1.569 ( 2.300) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.087 ( 0.140) | 1.155 ( 0.505) | 1.09- 0.96 | 44 | 1.063 ( 0.105) | 1.084 ( 0.143) | 1.117 ( 0.479) | 0.96- 0.84 | 44 | 1.073 ( 0.111) | 1.056 ( 0.136) | 1.145 ( 0.403) | 0.84- 0.81 | 44 | 1.112 ( 0.099) | 1.034 ( 0.130) | 1.356 ( 0.480) | 0.81- 0.73 | 44 | 1.088 ( 0.089) | 0.989 ( 0.129) | 1.292 ( 0.473) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.949 ( 0.114) | 1.392 ( 0.483) | 0.70- 0.67 | 44 | 1.077 ( 0.072) | 0.883 ( 0.071) | 1.434 ( 0.478) | 0.67- 0.63 | 44 | 1.073 ( 0.063) | 0.870 ( 0.063) | 1.462 ( 0.599) | 0.63- 0.59 | 44 | 1.010 ( 0.080) | 0.807 ( 0.036) | 1.264 ( 0.487) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 440 | 1.064 ( 0.108) | 1.005 ( 0.282) | 1.319 ( 0.875) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.960 ( 0.119) | 1.077 ( 0.432) | 0.75- 0.71 | 47 | 0.977 ( 0.042) | 0.911 ( 0.060) | 1.229 ( 0.520) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.858 ( 0.052) | 1.246 ( 0.476) | 0.66- 0.62 | 47 | 0.929 ( 0.045) | 0.841 ( 0.039) | 1.148 ( 0.407) | 0.62- 0.59 | 48 | 0.904 ( 0.043) | 0.810 ( 0.035) | 1.356 ( 0.591) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 471 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 470 obs out of 471 (total:471,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079674 -0.015486 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000013 0.000011 0.000009 ) -0.036211 -0.003638 0.076594 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032955 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.652) | 1.105 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 49 | 1.018 ( 0.076) | 1.021 ( 0.106) | 1.085 ( 0.441) | 0.92- 0.82 | 48 | 1.001 ( 0.082) | 0.980 ( 0.110) | 1.110 ( 0.379) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.963 ( 0.114) | 1.085 ( 0.438) | 0.75- 0.71 | 48 | 0.985 ( 0.046) | 0.917 ( 0.069) | 1.218 ( 0.499) | 0.71- 0.67 | 48 | 0.952 ( 0.047) | 0.863 ( 0.057) | 1.215 ( 0.481) | 0.66- 0.62 | 48 | 0.935 ( 0.047) | 0.847 ( 0.039) | 1.198 ( 0.425) | 0.62- 0.59 | 49 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.369 ( 0.581) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 478 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.996 ( 0.044) | 0.883 ( 0.075) | 1.182 ( 0.457) | 0.67- 0.62 | 47 | 0.976 ( 0.046) | 0.844 ( 0.040) | 1.294 ( 0.493) | 0.62- 0.59 | 47 | 0.948 ( 0.046) | 0.811 ( 0.043) | 1.357 ( 0.528) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 470 | 1.016 ( 0.092) | 0.989 ( 0.270) | 1.170 ( 0.535) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb PROFFITPEAK info: 980 peaks in the peak location table UB fit with 403 obs out of 454 (total:454,skipped:0) (88.77%) UB - matrix: -0.025194 -0.079416 -0.015659 ( 0.000033 0.000026 0.000022 ) 0.072495 -0.029385 0.032828 ( 0.000054 0.000042 0.000036 ) -0.036046 -0.003562 0.076519 ( 0.000033 0.000026 0.000022 ) M - matrix: 0.007190 -0.000001 0.000016 ( 0.000008 0.000004 0.000004 ) -0.000001 0.007183 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000016 0.000006 0.007178 ( 0.000004 0.000003 0.000004 ) unit cell: 8.365(4) 8.369(3) 8.372(3) 90.05(3) 90.13(3) 89.99(3) V = 586.1(4) UB fit with 403 obs out of 454 (total:454,skipped:0) (88.77%) UB - matrix: -0.025194 -0.079416 -0.015659 ( 0.000033 0.000026 0.000022 ) 0.072495 -0.029385 0.032828 ( 0.000054 0.000042 0.000036 ) -0.036046 -0.003562 0.076519 ( 0.000033 0.000026 0.000022 ) M - matrix: 0.007190 -0.000001 0.000016 ( 0.000008 0.000004 0.000004 ) -0.000001 0.007183 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000016 0.000006 0.007178 ( 0.000004 0.000003 0.000004 ) unit cell: 8.365(4) 8.369(3) 8.372(3) 90.05(3) 90.13(3) 89.99(3) V = 586.1(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB fit with 409 obs out of 454 (total:454,skipped:0) (90.09%) UB - matrix: -0.025232 -0.079424 -0.015689 ( 0.000034 0.000027 0.000023 ) 0.072507 -0.029408 0.032813 ( 0.000052 0.000041 0.000035 ) -0.036046 -0.003538 0.076542 ( 0.000034 0.000027 0.000023 ) M - matrix: 0.007193 -0.000001 0.000016 ( 0.000008 0.000004 0.000004 ) -0.000001 0.007186 0.000010 ( 0.000004 0.000005 0.000003 ) 0.000016 0.000010 0.007181 ( 0.000004 0.000003 0.000004 ) unit cell: 8.363(4) 8.368(3) 8.370(3) 90.08(3) 90.13(3) 89.99(3) V = 585.7(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 454 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 589 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025234 -0.079426 -0.015691 ( 0.000034 0.000027 0.000023 ) 0.072507 -0.029408 0.032813 ( 0.000052 0.000041 0.000035 ) -0.036046 -0.003536 0.076545 ( 0.000034 0.000027 0.000023 ) M - matrix: 0.007193 -0.000001 0.000016 ( 0.000008 0.000004 0.000004 ) -0.000001 0.007186 0.000011 ( 0.000004 0.000005 0.000003 ) 0.000016 0.000011 0.007182 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025234 -0.079426 -0.015691 ( 0.000034 0.000027 0.000023 ) 0.072507 -0.029408 0.032813 ( 0.000052 0.000041 0.000035 ) -0.036046 -0.003536 0.076545 ( 0.000034 0.000027 0.000023 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000002 ) UB fit with 409 obs out of 454 (total:454,skipped:0) (90.09%) unit cell: 8.363(4) 8.367(3) 8.370(3) 90.08(3) 90.13(3) 89.99(3) V = 585.7(4) unit cell: 8.3667(9) 8.3667(9) 8.3667(9) 90.0 90.0 90.0 V = 585.69(11) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 405 obs out of 454 (total:454,skipped:0) (89.21%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb 4 of 339 peaks identified as outliers and rejected 335 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 335 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 335 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.47 | 34 | 1.010 ( 0.156) | 1.205 ( 0.595) | 1.183 ( 0.836) | 1.47- 1.17 | 34 | 0.996 ( 0.119) | 1.156 ( 0.476) | 1.043 ( 0.580) | 1.17- 1.01 | 34 | 1.017 ( 0.082) | 1.099 ( 0.100) | 0.948 ( 0.388) | 1.01- 0.92 | 34 | 0.995 ( 0.088) | 1.039 ( 0.152) | 0.973 ( 0.379) | 0.92- 0.82 | 34 | 1.004 ( 0.081) | 1.021 ( 0.125) | 1.051 ( 0.364) | 0.82- 0.75 | 34 | 0.984 ( 0.066) | 0.972 ( 0.105) | 1.095 ( 0.450) | 0.75- 0.71 | 34 | 0.963 ( 0.054) | 0.904 ( 0.098) | 1.272 ( 0.503) | 0.71- 0.67 | 34 | 0.949 ( 0.045) | 0.883 ( 0.053) | 1.183 ( 0.423) | 0.66- 0.62 | 34 | 0.922 ( 0.042) | 0.842 ( 0.061) | 1.328 ( 0.472) | 0.62- 0.59 | 29 | 0.902 ( 0.048) | 0.820 ( 0.045) | 1.397 ( 0.527) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 335 | 0.975 ( 0.093) | 0.997 ( 0.287) | 1.144 ( 0.528) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) UB - matrix: -0.025255 -0.079586 -0.015510 ( 0.000023 0.000017 0.000017 ) 0.072574 -0.029393 0.032815 ( 0.000023 0.000017 0.000017 ) -0.036139 -0.003563 0.076577 ( 0.000017 0.000012 0.000013 ) M - matrix: 0.007211 0.000006 0.000006 ( 0.000004 0.000002 0.000002 ) 0.000006 0.007211 -0.000003 ( 0.000002 0.000003 0.000002 ) 0.000006 -0.000003 0.007181 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3529(19) 8.3531(18) 8.3700(15) 89.976(16) 90.046(16) 90.044(18) V = 584.0(2) OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 No constraint UB - matrix: -0.025302 -0.079390 -0.015690 ( 0.000015 0.000011 0.000011 ) 0.072406 -0.029462 0.032803 ( 0.000023 0.000017 0.000017 ) -0.036083 -0.003546 0.076605 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007185 0.000003 0.000008 ( 0.000004 0.000002 0.000002 ) 0.000003 0.007183 0.000008 ( 0.000002 0.000002 0.000001 ) 0.000008 0.000008 0.007191 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025302 -0.079390 -0.015690 ( 0.000015 0.000011 0.000011 ) 0.072406 -0.029462 0.032803 ( 0.000023 0.000017 0.000017 ) -0.036083 -0.003546 0.076605 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) unit cell: 8.3680(19) 8.3689(12) 8.3646(14) 90.060(13) 90.064(16) 90.028(15) V = 585.78(19) unit cell: 8.3672(4) 8.3672(4) 8.3672(4) 90.0 90.0 90.0 V = 585.78(5) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 590 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025302 -0.079390 -0.015690 ( 0.000015 0.000011 0.000011 ) 0.072406 -0.029462 0.032803 ( 0.000023 0.000017 0.000017 ) -0.036083 -0.003546 0.076605 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007185 0.000003 0.000008 ( 0.000004 0.000002 0.000002 ) 0.000003 0.007183 0.000008 ( 0.000002 0.000002 0.000001 ) 0.000008 0.000008 0.007191 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025302 -0.079390 -0.015690 ( 0.000015 0.000011 0.000011 ) 0.072406 -0.029462 0.032803 ( 0.000023 0.000017 0.000017 ) -0.036083 -0.003546 0.076605 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) unit cell: 8.3680(19) 8.3689(12) 8.3646(14) 90.060(13) 90.064(16) 90.028(15) V = 585.78(19) unit cell: 8.3672(4) 8.3672(4) 8.3672(4) 90.0 90.0 90.0 V = 585.78(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb 3 of 338 peaks identified as outliers and rejected 335 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 335 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 335 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.48 | 34 | 1.007 ( 0.155) | 1.204 ( 0.607) | 1.192 ( 0.834) | 1.48- 1.17 | 34 | 1.021 ( 0.102) | 1.201 ( 0.444) | 1.011 ( 0.550) | 1.17- 1.02 | 34 | 1.002 ( 0.089) | 1.069 ( 0.125) | 0.988 ( 0.391) | 1.01- 0.92 | 34 | 1.009 ( 0.090) | 1.080 ( 0.146) | 0.932 ( 0.442) | 0.92- 0.82 | 34 | 0.991 ( 0.083) | 1.003 ( 0.122) | 1.054 ( 0.374) | 0.82- 0.75 | 34 | 0.985 ( 0.065) | 0.973 ( 0.108) | 1.123 ( 0.442) | 0.75- 0.71 | 34 | 0.962 ( 0.053) | 0.911 ( 0.101) | 1.323 ( 0.498) | 0.71- 0.67 | 34 | 0.943 ( 0.047) | 0.878 ( 0.048) | 1.145 ( 0.403) | 0.66- 0.62 | 34 | 0.922 ( 0.042) | 0.843 ( 0.061) | 1.327 ( 0.469) | 0.62- 0.59 | 29 | 0.902 ( 0.049) | 0.819 ( 0.041) | 1.395 ( 0.541) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 335 | 0.976 ( 0.093) | 1.001 ( 0.288) | 1.145 ( 0.531) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 258 | 1.116 ( 0.130) | 1.237 ( 0.476) | 1.253 ( 1.105) | 13.0-18.7 | 258 | 1.075 ( 0.053) | 1.126 ( 0.229) | 1.169 ( 0.510) | 18.8-22.9 | 258 | 1.063 ( 0.068) | 1.141 ( 0.382) | 1.163 ( 0.548) | 22.9-27.1 | 258 | 1.030 ( 0.074) | 1.065 ( 0.239) | 1.137 ( 0.530) | 27.1-30.6 | 258 | 1.008 ( 0.073) | 1.017 ( 0.271) | 1.209 ( 0.496) | 30.6-33.8 | 258 | 0.976 ( 0.077) | 0.929 ( 0.095) | 1.187 ( 0.517) | 33.8-37.0 | 258 | 0.956 ( 0.072) | 0.905 ( 0.119) | 1.160 ( 0.475) | 37.0-39.7 | 258 | 0.938 ( 0.083) | 0.868 ( 0.126) | 1.215 ( 0.549) | 39.7-42.7 | 258 | 0.920 ( 0.075) | 0.839 ( 0.092) | 1.199 ( 0.545) | 42.7-49.9 | 262 | 0.922 ( 0.084) | 0.813 ( 0.073) | 1.155 ( 0.476) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2584 | 1.000 ( 0.104) | 0.994 ( 0.282) | 1.185 ( 0.603) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0096 b=1.25 e3 dimension: a=0.0020 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28155044 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 15:54:45 2018 PROFFITMAIN - Started at Tue Mar 27 15:54:45 2018 OTKP changes: 2577 2 4 6 OTKP changes: 2577 2 4 6 No constraint UB - matrix: -0.025033 -0.079527 -0.015589 ( 0.000006 0.000006 0.000006 ) 0.072515 -0.029217 0.032947 ( 0.000005 0.000006 0.000006 ) -0.036231 -0.003595 0.076551 ( 0.000004 0.000005 0.000004 ) M - matrix: 0.007198 0.000002 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007191 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000002 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025033 -0.079527 -0.015589 ( 0.000006 0.000006 0.000006 ) 0.072515 -0.029217 0.032947 ( 0.000005 0.000006 0.000006 ) -0.036231 -0.003595 0.076551 ( 0.000004 0.000005 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) UB fit with 2580 obs out of 2584 (total:2584,skipped:0) (99.85%) unit cell: 8.3605(5) 8.3644(6) 8.3658(4) 90.016(5) 90.046(5) 90.019(5) V = 585.02(6) unit cell: 8.36355(15) 8.36355(15) 8.36355(15) 90.0 90.0 90.0 V = 585.022(18) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028809 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036122 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024871 -0.079573 -0.015661 ( 0.000013 0.000015 0.000011 ) 0.072447 -0.029202 0.032953 ( 0.000016 0.000018 0.000013 ) -0.036289 -0.003652 0.076365 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000004 0.000006 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007198 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000006 0.000005 0.007163 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3684(15) 8.3604(15) 8.3809(10) 90.040(12) 90.045(12) 89.968(14) V = 586.35(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024978 -0.079529 -0.015506 ( 0.000017 0.000014 0.000012 ) 0.072508 -0.029253 0.033012 ( 0.000012 0.000010 0.000008 ) -0.036257 -0.003632 0.076504 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000007 -0.000010 0.007183 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3616(11) 8.3628(14) 8.3690(11) 89.917(12) 90.057(11) 89.977(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3568(14) 8.3623(11) 89.937(12) 90.002(11) 89.958(12) V = 583.91(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.91(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3568(14) 8.3623(11) 89.937(12) 90.002(11) 89.958(12) V = 583.91(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.91(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072548 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036287 -0.003566 0.076599 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3568(14) 8.3623(11) 89.937(12) 90.002(11) 89.958(12) V = 583.91(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.91(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 470 obs out of 470 (total:470,skipped:0) (100.00%) UB - matrix: -0.025008 -0.079543 -0.015713 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029339 0.032913 ( 0.000009 0.000014 0.000014 ) -0.036184 -0.003658 0.076519 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007179 -0.000003 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007201 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000008 0.000004 0.007185 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3714(11) 8.3584(12) 8.3677(11) 90.034(11) 90.061(11) 89.975(11) V = 585.50(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 470 obs out of 470 (total:470,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3594(11) 89.996(11) 90.020(10) 90.031(11) V = 584.33(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.33(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 470 obs out of 470 (total:470,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3594(11) 89.996(11) 90.020(10) 90.031(11) V = 584.33(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.33(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 470 obs out of 470 (total:470,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015723 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003692 0.076579 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 470 obs out of 470 (total:470,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3594(11) 89.996(11) 90.020(10) 90.031(11) V = 584.33(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.33(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025236 -0.079450 -0.015776 ( 0.000011 0.000016 0.000017 ) 0.072345 -0.029412 0.032796 ( 0.000008 0.000011 0.000012 ) -0.036271 -0.003613 0.076596 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007190 0.000012 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000012 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3672(10) 8.3648(14) 8.3642(11) 90.097(13) 89.940(10) 90.066(12) V = 585.40(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.03(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.03(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.03(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.03(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.03(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.03(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) UB - matrix: -0.025297 -0.079460 -0.015623 ( 0.000017 0.000013 0.000013 ) 0.072460 -0.029411 0.032823 ( 0.000023 0.000017 0.000017 ) -0.036097 -0.003532 0.076573 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007193 0.000007 0.000010 ( 0.000004 0.000002 0.000002 ) 0.000007 0.007191 0.000006 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000006 0.007185 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3631(19) 8.3642(14) 8.3680(14) 90.044(14) 90.076(16) 90.052(16) V = 585.3(2) OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 OTKP changes: 334 1 1 1 No constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007198 0.000003 0.000009 ( 0.000004 0.000002 0.000002 ) 0.000003 0.007195 0.000007 ( 0.000002 0.000002 0.000002 ) 0.000009 0.000007 0.007206 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) unit cell: 8.3603(19) 8.3620(13) 8.3558(14) 90.057(13) 90.073(16) 90.023(15) V = 584.14(19) unit cell: 8.3594(4) 8.3594(4) 8.3594(4) 90.0 90.0 90.0 V = 584.14(5) Run 6 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.757) HKL list info: 578 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007198 0.000003 0.000009 ( 0.000004 0.000002 0.000002 ) 0.000003 0.007195 0.000007 ( 0.000002 0.000002 0.000002 ) 0.000009 0.000007 0.007206 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) unit cell: 8.3603(19) 8.3620(13) 8.3558(14) 90.057(13) 90.073(16) 90.023(15) V = 584.14(19) unit cell: 8.3594(4) 8.3594(4) 8.3594(4) 90.0 90.0 90.0 V = 584.14(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007198 0.000003 0.000009 ( 0.000004 0.000002 0.000002 ) 0.000003 0.007195 0.000007 ( 0.000002 0.000002 0.000002 ) 0.000009 0.000007 0.007206 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025294 -0.079459 -0.015729 ( 0.000015 0.000011 0.000012 ) 0.072494 -0.029471 0.032822 ( 0.000023 0.000017 0.000018 ) -0.036095 -0.003590 0.076689 ( 0.000016 0.000012 0.000012 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000001 ) UB fit with 334 obs out of 335 (total:335,skipped:0) (99.70%) unit cell: 8.3603(19) 8.3620(13) 8.3558(14) 90.057(13) 90.073(16) 90.023(15) V = 584.14(19) unit cell: 8.3594(4) 8.3594(4) 8.3594(4) 90.0 90.0 90.0 V = 584.14(5) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025021 -0.079452 -0.015565 ( 0.000006 0.000007 0.000006 ) 0.072509 -0.029189 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036230 -0.003592 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 0.000002 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007177 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000001 0.007185 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025021 -0.079452 -0.015565 ( 0.000006 0.000007 0.000006 ) 0.072509 -0.029189 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036230 -0.003592 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) UB fit with 2580 obs out of 2584 (total:2584,skipped:0) (99.85%) unit cell: 8.3614(6) 8.3723(6) 8.3679(5) 90.009(5) 90.018(5) 90.013(6) V = 585.79(7) unit cell: 8.36721(19) 8.36721(19) 8.36721(19) 90.0 90.0 90.0 V = 585.79(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 71 reflections under beam stop or inside a detector rejection region 23 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3489 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 15:54:53 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) Run 6 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.757) PROFFIT INFO: signal sum: min=255.0000 max=22950984.0000 PROFFIT INFO: signal sum lp corr: min=469.4961 max=3201279.8420 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=462 PROFFIT INFO: Inet: min=751.1938 max=5122047.5000 PROFFIT INFO: sig(Inet): min=120.3459 max=47790.0820 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 39 166 367 709 796 1439 2327 3201 3489 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.2 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3489 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3489 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5122048- 1128457 348 1876049.89 121.23 100.00 1124326- 621839 348 848209.00 102.65 100.00 620665- 265839 348 414090.05 94.89 100.00 264444- 169807 348 203524.57 71.81 100.00 169654- 120034 348 144654.27 51.16 100.00 119658- 92250 348 105122.24 35.79 100.00 92187- 65637 348 80018.94 29.11 100.00 65554- 5569 348 37526.17 19.27 100.00 5541- 2986 348 3942.15 5.38 97.70 2983- 751 357 2140.99 3.72 55.74 ------------------------------------------------------------------------------------ 5122048- 751 3489 370574.98 53.37 95.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 756499.68 94.28 100.00 1.41- 1.12 348 610638.19 62.66 99.43 1.12- 0.96 348 510672.41 71.11 97.99 0.96- 0.88 348 347752.85 59.70 94.54 0.88- 0.81 348 450393.56 68.75 99.43 0.81- 0.73 348 249128.77 41.55 95.40 0.73- 0.71 348 175107.11 34.49 89.66 0.71- 0.65 348 309231.58 47.12 93.39 0.65- 0.62 348 153438.56 27.28 87.93 0.62- 0.58 357 148627.12 27.47 94.68 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 370574.98 53.37 95.24 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:54:53 2018 Sorting 3489 observations 119 unique observations with > 7.00 F2/sig(F2) 3489 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 74 596 Total number of frames 596 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3489 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 12 102 Total number of frames 102 2802 observations > 7.00 F2/sig(F2) 2802 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 12 102 Total number of frames 102 Removing 'redundancy=1' reflections Average redundancy: 21.7 (Out of 2802 removed 4 = 2798, unique = 129) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2798 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 12 102 Total number of frames 102 129 unique data precomputed (should be 129) 129 unique data with 2798 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 21.7 (Out of 2798 removed 0 = 2798, unique = 129) 129 unique data precomputed (should be 129) 129 unique data with 2798 observations RMS deviation of equivalent data = 0.25493 Rint = 0.18526 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17785, wR= 0.26150 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13510, wR= 0.17134, Acormin=0.609, Acormax=1.414, Acor_av=0.991 F test: Probability=1.000, F= 1.730 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12125, wR= 0.15003, Acormin=0.554, Acormax=1.442, Acor_av=0.910 F test: Probability=1.000, F= 1.240 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10817, wR= 0.14234, Acormin=0.653, Acormax=1.599, Acor_av=0.982 F test: Probability=1.000, F= 1.253 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09345, wR= 0.12256, Acormin=0.536, Acormax=1.558, Acor_av=0.899 F test: Probability=1.000, F= 1.338 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08105, wR= 0.11030, Acormin=0.518, Acormax=1.625, Acor_av=0.913 F test: Probability=1.000, F= 1.326 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09966, wR= 0.13493, Acormin=0.643, Acormax=1.671, Acor_av=0.986 F test: Probability=0.000, F= 0.661 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08690, wR= 0.11670, Acormin=0.518, Acormax=1.631, Acor_av=0.906 F test: Probability=0.000, F= 0.868 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07686, wR= 0.10675, Acormin=0.503, Acormax=1.659, Acor_av=0.917 F test: Probability=0.995, F= 1.107 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07360, wR= 0.10100, Acormin=0.393, Acormax=1.544, Acor_av=0.872 F test: Probability=0.982, F= 1.086 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10014, wR= 0.13083, Acormin=0.491, Acormax=1.487, Acor_av=0.853 F test: Probability=0.000, F= 0.541 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08501, wR= 0.11215, Acormin=0.511, Acormax=1.629, Acor_av=0.895 F test: Probability=0.000, F= 0.750 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08347, wR= 0.10985, Acormin=0.115, Acormax=0.418, Acor_av=0.226 F test: Probability=0.000, F= 0.776 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07521, wR= 0.10113, Acormin=0.116, Acormax=0.441, Acor_av=0.250 F test: Probability=0.000, F= 0.951 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07008, wR= 0.09449, Acormin=0.126, Acormax=0.461, Acor_av=0.262 F test: Probability=0.985, F= 1.089 Final absorption model (ne=6, no=5): Rint= 0.07360, Acormin=0.393, Acormax=1.544, Acor_av=0.872 Combined refinement in use Rint: 0.18537 There are 102 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 149 pars with 11175 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25493 Using Levenberg-Marquardt: 0.00010 New wR= 0.06354 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18526 with corrections 0.05129 Rint for all data: 0.18537 with corrections 0.05152 0 observations identified as outliers and rejected Cycle 2 wR= 0.06354 Using Levenberg-Marquardt: 0.00001 New wR= 0.06049 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18526 with corrections 0.04847 Rint for all data: 0.18537 with corrections 0.04870 0 observations identified as outliers and rejected Cycle 3 wR= 0.06049 Using Levenberg-Marquardt: 0.00000 New wR= 0.05988 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18526 with corrections 0.04793 Rint for all data: 0.18537 with corrections 0.04816 0 observations identified as outliers and rejected Cycle 4 wR= 0.05988 Using Levenberg-Marquardt: 0.00000 New wR= 0.05958 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18526 with corrections 0.04766 Rint for all data: 0.18537 with corrections 0.04789 0 observations identified as outliers and rejected Cycle 5 wR= 0.05958 Using Levenberg-Marquardt: 0.00000 New wR= 0.05939 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18526 with corrections 0.04749 Rint for all data: 0.18537 with corrections 0.04772 0 observations identified as outliers and rejected Final wR= 0.05939 Final frame scales: Min= 0.7700 Max= 1.3559 Final absorption correction factors: Amin= 0.4864 Amax= 1.4298 PROFFIT INFO: Inet (after scale3 abspack): min=751.5054 max=4617534.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=144.6917 max=53029.2344 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3489 reflections read from tmp file 773 reflections are rejected (772 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 4 5 4 1 3 7 6 122 Initial Chi^2= 0.44021 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.97374 Current error model SIG(F2)^2 = 167.54*I_RAW + 0.00*I_BACK+(0.01375*)^2 Cycle 2, Chi^2= 1.03186 Current error model SIG(F2)^2 = 104.68*I_RAW + 0.00*I_BACK+(0.02282*)^2 Cycle 3, Chi^2= 1.00142 Current error model SIG(F2)^2 = 121.54*I_RAW + 0.00*I_BACK+(0.01996*)^2 Cycle 4, Chi^2= 0.99996 Current error model SIG(F2)^2 = 119.63*I_RAW + 0.00*I_BACK+(0.02042*)^2 Cycle 5, Chi^2= 1.00002 Current error model SIG(F2)^2 = 120.05*I_RAW + 0.00*I_BACK+(0.02032*)^2 Cycle 6, Chi^2= 1.00000 Current error model SIG(F2)^2 = 119.97*I_RAW + 0.00*I_BACK+(0.02034*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 119.97*I_RAW + 0.00*I_BACK+(0.02034*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4617535- 1087947 348 1767984.91 45.52 100.00 1087574- 604204 348 809522.22 37.89 100.00 603967- 256068 348 402669.61 36.43 100.00 256051- 153699 348 192589.05 31.77 100.00 153681- 124177 348 139234.37 25.55 100.00 124106- 87290 348 101753.91 19.43 100.00 87129- 67915 348 78030.28 16.71 100.00 67901- 5001 348 39609.62 12.02 100.00 4996- 2755 348 3636.24 4.58 95.69 2755- 752 357 2147.62 3.73 74.23 ------------------------------------------------------------------------------------ 4617535- 752 3489 352810.90 23.31 96.93 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 755013.62 37.24 100.00 1.41- 1.12 348 588526.23 29.00 99.43 1.12- 0.96 348 470151.42 27.99 98.56 0.96- 0.88 348 327173.07 23.92 97.13 0.88- 0.81 348 425699.78 27.36 99.71 0.81- 0.73 348 228895.63 18.95 96.26 0.73- 0.71 348 166145.69 17.49 91.67 0.71- 0.65 348 290471.09 22.15 97.99 0.65- 0.62 348 144109.42 14.41 91.95 0.62- 0.58 357 137491.61 14.83 96.64 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 352810.90 23.31 96.93 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 755013.62 37.24 100.00 4.82- 1.12 696 671769.92 33.12 99.71 4.82- 0.96 1044 604563.76 31.41 99.33 4.82- 0.88 1392 535216.08 29.54 98.78 4.82- 0.81 1740 513312.82 29.10 98.97 4.82- 0.73 2088 465909.96 27.41 98.52 4.82- 0.71 2436 423086.49 25.99 97.54 4.82- 0.65 2784 406509.57 25.51 97.59 4.82- 0.62 3132 377353.99 24.28 96.97 4.82- 0.58 3489 352810.90 23.31 96.93 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 352810.90 23.31 96.93 Scale applied to data: s=0.216566 (maximum obs:4617534.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.028: data 3489 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.028: data 3479 -> merged 157 Rejected total: 10, method kkm 10, method Blessing 0 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585822, 4.830812 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 20.29 100.00 284 1.41 - 1.12 14 14 28.71 100.00 402 1.12 - 0.97 14 14 28.50 100.00 399 0.96 - 0.84 14 14 30.43 100.00 426 0.84 - 0.78 14 14 23.57 100.00 330 0.78 - 0.73 14 14 24.64 100.00 345 0.73 - 0.69 14 14 22.79 100.00 319 0.69 - 0.66 14 14 19.50 100.00 273 0.65 - 0.63 14 14 20.43 100.00 286 0.63 - 0.60 14 14 17.86 100.00 250 --------------------------------------------------------------- 8.36 - 0.60 140 140 23.67 100.00 3314 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:54:54 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361414 8.372288 8.367937 90.0091 90.0179 90.0128 3479 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.32 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1780 0 2336 2333 3479 N (int>3sigma) = 0 0 0 0 1780 0 2266 2258 3372 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 76.9 78.9 76.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 585.79 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.914 5.916 5.916 119.97 90.04 119.95 Niggli form: a.a = 34.973 b.b = 34.994 c.c = 34.995 b.c = -17.483 a.c = -0.027 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.055 CUBIC F-lattice R(int) = 0.047 [ 3322] Vol = 585.8 Cell: 8.361 8.372 8.368 89.99 89.98 90.01 Volume: 585.79 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.053 [ 3043] Vol = 439.3 Cell: 5.916 5.914 14.494 89.97 90.05 119.95 Volume: 439.34 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 970] Vol = 439.3 Trigonal Cell: 5.916 5.914 14.494 89.97 90.05 119.95 Volume: 439.34 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.046 [ 3071] Vol = 292.9 Cell: 5.919 5.918 8.361 89.98 90.00 90.03 Volume: 292.90 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.046 TETRAGONAL I-lattice R(int) = 0.046 [ 3071] Vol = 292.9 Cell: 5.919 5.918 8.361 89.98 90.00 90.03 Volume: 292.90 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 3018] Vol = 292.9 Cell: 5.919 8.361 5.918 89.98 89.97 90.00 Volume: 292.90 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.045 [ 2668] Vol = 292.9 Cell: 8.361 5.919 5.918 90.03 90.02 90.00 Volume: 292.90 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.034 MONOCLINIC I-lattice R(int) = 0.044 [ 2672] Vol = 292.9 Cell: 5.916 5.914 8.372 89.98 90.00 89.96 Volume: 292.90 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.019 MONOCLINIC C-lattice R(int) = 0.044 [ 2681] Vol = 292.9 Cell: 8.361 8.372 5.914 89.98 134.97 90.01 Volume: 292.90 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2011] Vol = 146.4 Cell: 5.914 5.916 5.916 119.97 90.04 119.95 Volume: 146.45 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1780 0 2333 2336 3479 N (int>3sigma) = 0 0 0 0 1780 0 2258 2266 3372 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 78.9 76.9 76.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.5 23.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.179 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 260 778 N I>3s 37 37 247 778 1.0 1.0 0.7 36.3 8.9 8.9 5.3 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3082 Fd-3m 1 1 227 C N N N N 37 2284 0.048 3121 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361414 8.372288 8.367937 89.9909 89.9821 90.0128 ZERR 3.00 0.000599 0.000650 0.000491 0.0055 0.0053 0.0060 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4006260- 748937 568 566 26 21.8 1427825.08 43.05 0.041 0.056 737983- 224516 541 540 26 20.8 448098.08 36.51 0.063 0.081 219447- 96631 811 811 26 31.2 147819.32 26.21 0.043 0.055 93987- 69388 556 554 26 21.3 81798.05 16.89 0.071 0.090 64630- 3587 455 453 26 17.4 26050.46 9.06 0.087 0.111 3441- 1717 558 555 27 20.6 2660.22 4.20 0.200 0.259 ------------------------------------------------------------------------------------------- 4006260- 1717 3489 3479 157 22.2 353146.55 23.32 0.047 0.063 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 652 648 26 24.9 615107.38 32.38 0.049 0.066 0.022 1.12-0.88 766 765 26 29.4 458227.20 27.18 0.033 0.045 0.025 0.85-0.75 651 651 26 25.0 325061.53 22.69 0.042 0.053 0.029 0.74-0.68 566 564 26 21.7 252522.06 20.21 0.059 0.068 0.033 0.67-0.63 537 537 26 20.7 148572.57 15.97 0.078 0.095 0.042 0.62-0.59 317 314 27 11.6 145358.23 14.70 0.078 0.087 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3489 3479 157 22.2 353146.55 23.32 0.047 0.063 0.028 inf-0.60 3321 3312 139 23.8 365563.62 23.82 0.047 0.062 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 648 26 26 100.0 24.9 615107.38 175.41 0.049 0.006 1.12-0.88 765 26 26 100.0 29.4 458227.20 149.84 0.033 0.005 0.85-0.75 651 26 26 100.0 25.0 325061.53 120.15 0.042 0.006 0.74-0.68 564 26 26 100.0 21.7 252522.06 96.21 0.059 0.008 0.67-0.63 537 26 26 100.0 20.7 148572.57 71.96 0.078 0.009 0.62-0.59 314 27 27 100.0 11.6 145358.23 58.48 0.078 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3479 157 157 100.0 22.2 353146.55 120.08 0.047 0.007 inf-0.60 3312 139 139 100.0 23.8 365563.62 123.72 0.047 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025021 -0.079452 -0.015565 ( 0.000006 0.000007 0.000006 ) 0.072509 -0.029189 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036230 -0.003592 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 0.000002 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007177 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000001 0.007185 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025021 -0.079452 -0.015565 ( 0.000006 0.000007 0.000006 ) 0.072509 -0.029189 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036230 -0.003592 0.076549 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007186 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007186 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007186 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3614(6) 8.3723(6) 8.3679(5) 90.009(5) 90.018(5) 90.013(6) V = 585.79(7) unit cell: 8.36721(19) 8.36721(19) 8.36721(19) 90.0 90.0 90.0 V = 585.79(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) Run 6 Omega scan: (-1.000 - 74.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.757) PROFFIT INFO: signal sum: min=255.0000 max=22950984.0000 PROFFIT INFO: signal sum lp corr: min=469.4961 max=3201279.8420 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=545.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=462 PROFFIT INFO: Inet: min=751.1938 max=5122047.5000 PROFFIT INFO: sig(Inet): min=120.3459 max=47790.0820 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.81 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 78 332 734 1418 1592 2878 4654 6402 6978 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.2 66.7 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3489 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3489 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5122048- 1128457 348 1876049.89 121.23 100.00 1124326- 621839 348 848209.00 102.65 100.00 620665- 265839 348 414090.05 94.89 100.00 264444- 169807 348 203524.57 71.81 100.00 169654- 120034 348 144654.27 51.16 100.00 119658- 92250 348 105122.24 35.79 100.00 92187- 65637 348 80018.94 29.11 100.00 65554- 5569 348 37526.17 19.27 100.00 5541- 2986 348 3942.15 5.38 97.70 2983- 751 357 2140.99 3.72 55.74 ------------------------------------------------------------------------------------ 5122048- 751 3489 370574.98 53.37 95.24 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 756499.68 94.28 100.00 1.41- 1.12 348 610638.19 62.66 99.43 1.12- 0.96 348 510672.41 71.11 97.99 0.96- 0.88 348 347752.85 59.70 94.54 0.88- 0.81 348 450393.56 68.75 99.43 0.81- 0.73 348 249128.77 41.55 95.40 0.73- 0.71 348 175107.11 34.49 89.66 0.71- 0.65 348 309231.58 47.12 93.39 0.65- 0.62 348 153438.56 27.28 87.93 0.62- 0.58 357 148627.12 27.47 94.68 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 370574.98 53.37 95.24 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 15:54:55 2018 Sorting 3489 observations 86 unique observations with > 7.00 F2/sig(F2) 3489 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 74 596 Total number of frames 596 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 3489 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 10 89 Total number of frames 89 2802 observations > 7.00 F2/sig(F2) 2802 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 10 89 Total number of frames 89 Removing 'redundancy=1' reflections Average redundancy: 30.1 (Out of 2802 removed 3 = 2799, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2799 observations in 6 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 10 89 Total number of frames 89 93 unique data precomputed (should be 93) 93 unique data with 2799 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 30.1 (Out of 2799 removed 0 = 2799, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2799 observations RMS deviation of equivalent data = 0.25527 Rint = 0.18552 10 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17718, wR= 0.26009 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13486, wR= 0.17155, Acormin=0.610, Acormax=1.412, Acor_av=0.991 F test: Probability=1.000, F= 1.723 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12159, wR= 0.15069, Acormin=0.554, Acormax=1.442, Acor_av=0.910 F test: Probability=1.000, F= 1.229 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10824, wR= 0.14266, Acormin=0.651, Acormax=1.597, Acor_av=0.982 F test: Probability=1.000, F= 1.259 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09351, wR= 0.12303, Acormin=0.537, Acormax=1.556, Acor_av=0.899 F test: Probability=1.000, F= 1.338 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08111, wR= 0.11094, Acormin=0.516, Acormax=1.624, Acor_av=0.912 F test: Probability=1.000, F= 1.326 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09944, wR= 0.13519, Acormin=0.642, Acormax=1.673, Acor_av=0.987 F test: Probability=0.000, F= 0.665 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08689, wR= 0.11702, Acormin=0.519, Acormax=1.633, Acor_av=0.907 F test: Probability=0.000, F= 0.869 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07689, wR= 0.10716, Acormin=0.505, Acormax=1.662, Acor_av=0.918 F test: Probability=0.996, F= 1.108 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07382, wR= 0.10153, Acormin=0.399, Acormax=1.547, Acor_av=0.874 F test: Probability=0.976, F= 1.080 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10009, wR= 0.13124, Acormin=0.500, Acormax=1.494, Acor_av=0.855 F test: Probability=0.000, F= 0.545 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08480, wR= 0.11237, Acormin=0.513, Acormax=1.636, Acor_av=0.896 F test: Probability=0.000, F= 0.758 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08364, wR= 0.11063, Acormin=0.115, Acormax=0.417, Acor_av=0.225 F test: Probability=0.000, F= 0.777 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07545, wR= 0.10204, Acormin=0.117, Acormax=0.438, Acor_av=0.248 F test: Probability=0.000, F= 0.951 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07035, wR= 0.09527, Acormin=0.125, Acormax=0.457, Acor_av=0.259 F test: Probability=0.985, F= 1.088 Final absorption model (ne=6, no=5): Rint= 0.07382, Acormin=0.399, Acormax=1.547, Acor_av=0.874 Combined refinement in use Rint: 0.18563 There are 89 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25527 Using Levenberg-Marquardt: 0.00010 New wR= 0.06425 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18552 with corrections 0.05174 Rint for all data: 0.18563 with corrections 0.05196 0 observations identified as outliers and rejected Cycle 2 wR= 0.06425 Using Levenberg-Marquardt: 0.00001 New wR= 0.06115 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18552 with corrections 0.04885 Rint for all data: 0.18563 with corrections 0.04907 0 observations identified as outliers and rejected Cycle 3 wR= 0.06115 Using Levenberg-Marquardt: 0.00000 New wR= 0.06042 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18552 with corrections 0.04811 Rint for all data: 0.18563 with corrections 0.04834 0 observations identified as outliers and rejected Cycle 4 wR= 0.06042 Using Levenberg-Marquardt: 0.00000 New wR= 0.06002 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18552 with corrections 0.04769 Rint for all data: 0.18563 with corrections 0.04792 0 observations identified as outliers and rejected Cycle 5 wR= 0.06002 Using Levenberg-Marquardt: 0.00000 New wR= 0.05976 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18552 with corrections 0.04741 Rint for all data: 0.18563 with corrections 0.04764 0 observations identified as outliers and rejected Final wR= 0.05976 Final frame scales: Min= 0.7406 Max= 1.2637 Final absorption correction factors: Amin= 0.4824 Amax= 1.4197 PROFFIT INFO: Inet (after scale3 abspack): min=752.2263 max=4623925.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=144.1689 max=53531.8828 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3489 reflections read from tmp file 778 reflections are rejected (778 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 3 2 0 2 2 5 4 88 Initial Chi^2= 0.40976 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.01548 Current error model SIG(F2)^2 = 162.61*I_RAW + 0.00*I_BACK+(0.01310*)^2 Cycle 2, Chi^2= 1.03383 Current error model SIG(F2)^2 = 101.19*I_RAW + 0.00*I_BACK+(0.02230*)^2 Cycle 3, Chi^2= 1.00119 Current error model SIG(F2)^2 = 118.11*I_RAW + 0.00*I_BACK+(0.01970*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 116.36*I_RAW + 0.00*I_BACK+(0.02008*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 116.71*I_RAW + 0.00*I_BACK+(0.02001*)^2 Cycle 6, Chi^2= 1.00000 Current error model SIG(F2)^2 = 116.64*I_RAW + 0.00*I_BACK+(0.02002*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 116.64*I_RAW + 0.00*I_BACK+(0.02002*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4623925- 1094519 348 1768722.86 46.25 100.00 1093732- 604503 348 810048.89 38.49 100.00 603984- 256922 348 402540.37 37.00 100.00 256914- 154129 348 192614.42 32.22 100.00 154072- 124191 348 139295.90 25.94 100.00 124164- 87242 348 101614.32 19.70 100.00 87237- 68151 348 78042.66 16.97 100.00 68144- 5001 348 39618.30 12.16 100.00 4949- 2754 348 3635.90 4.66 96.26 2745- 752 357 2152.12 3.77 75.63 ------------------------------------------------------------------------------------ 4623925- 752 3489 352921.41 23.66 97.13 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 754463.80 37.81 100.00 1.41- 1.12 348 589380.68 29.48 99.43 1.12- 0.96 348 470015.24 28.41 98.85 0.96- 0.88 348 327796.27 24.27 97.41 0.88- 0.81 348 426226.29 27.77 99.71 0.81- 0.73 348 229242.73 19.23 96.55 0.73- 0.71 348 166091.18 17.74 91.95 0.71- 0.65 348 290201.76 22.48 97.99 0.65- 0.62 348 144217.22 14.62 92.53 0.62- 0.58 357 137159.01 15.05 96.92 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 352921.41 23.66 97.13 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 348 754463.80 37.81 100.00 4.82- 1.12 696 671922.24 33.65 99.71 4.82- 0.96 1044 604619.90 31.90 99.43 4.82- 0.88 1392 535413.99 30.00 98.92 4.82- 0.81 1740 513576.45 29.55 99.08 4.82- 0.73 2088 466187.50 27.83 98.66 4.82- 0.71 2436 423316.60 26.39 97.70 4.82- 0.65 2784 406677.24 25.90 97.74 4.82- 0.62 3132 377515.02 24.65 97.16 4.82- 0.58 3489 352921.41 23.66 97.13 ------------------------------------------------------------------------------------ 4.82- 0.58 3489 352921.41 23.66 97.13 Scale applied to data: s=0.216266 (maximum obs:4623925.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.027: data 3489 -> merged 110 With outlier rejection... Rint 0.048; Rsigma 0.027: data 3483 -> merged 110 Rejected total: 6, method kkm 4, method Blessing 2 Completeness direct cell (a, b, c) = (8.367, 8.367, 8.367), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585822, 4.830813 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 21.40 100.00 214 1.61 - 1.21 10 10 32.40 100.00 324 1.17 - 1.01 10 10 41.20 100.00 412 0.99 - 0.89 10 10 40.30 100.00 403 0.88 - 0.81 10 10 38.80 100.00 388 0.81 - 0.74 10 10 33.80 100.00 338 0.73 - 0.71 10 10 36.80 100.00 368 0.70 - 0.66 10 10 30.90 100.00 309 0.66 - 0.64 10 10 28.80 100.00 288 0.63 - 0.60 10 10 27.30 100.00 273 --------------------------------------------------------------- 8.36 - 0.60 100 100 33.17 100.00 3317 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 15:54:54 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361414 8.372288 8.367937 90.0091 90.0179 90.0128 3479 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.32 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1780 0 2336 2333 3479 N (int>3sigma) = 0 0 0 0 1780 0 2266 2258 3372 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 76.9 78.9 76.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 585.79 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Unitcell: 5.914 5.916 5.916 119.97 90.04 119.95 Niggli form: a.a = 34.973 b.b = 34.994 c.c = 34.995 b.c = -17.483 a.c = -0.027 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.055 CUBIC F-lattice R(int) = 0.047 [ 3322] Vol = 585.8 Cell: 8.361 8.372 8.368 89.99 89.98 90.01 Volume: 585.79 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.053 [ 3043] Vol = 439.3 Cell: 5.916 5.914 14.494 89.97 90.05 119.95 Volume: 439.34 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.055 RHOMBOHEDRAL R-lattice R(int) = 0.043 [ 970] Vol = 439.3 Trigonal Cell: 5.916 5.914 14.494 89.97 90.05 119.95 Volume: 439.34 Matrix:-0.5000 -0.5000 0.0000 0.5000 0.0000 0.5000 -1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.046 [ 3071] Vol = 292.9 Cell: 5.919 5.918 8.361 89.98 90.00 90.03 Volume: 292.90 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.046 TETRAGONAL I-lattice R(int) = 0.046 [ 3071] Vol = 292.9 Cell: 5.919 5.918 8.361 89.98 90.00 90.03 Volume: 292.90 Matrix: 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.033 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 3018] Vol = 292.9 Cell: 5.919 8.361 5.918 89.98 89.97 90.00 Volume: 292.90 Matrix: 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.022 MONOCLINIC I-lattice R(int) = 0.045 [ 2668] Vol = 292.9 Cell: 8.361 5.919 5.918 90.03 90.02 90.00 Volume: 292.90 Matrix:-1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.034 MONOCLINIC I-lattice R(int) = 0.044 [ 2672] Vol = 292.9 Cell: 5.916 5.914 8.372 89.98 90.00 89.96 Volume: 292.90 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.019 MONOCLINIC C-lattice R(int) = 0.044 [ 2681] Vol = 292.9 Cell: 8.361 8.372 5.914 89.98 134.97 90.01 Volume: 292.90 Matrix:-1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2011] Vol = 146.4 Cell: 5.914 5.916 5.916 119.97 90.04 119.95 Volume: 146.45 Matrix: 0.5000 0.0000 0.5000 -0.5000 -0.5000 0.0000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1780 0 2333 2336 3479 N (int>3sigma) = 0 0 0 0 1780 0 2258 2266 3372 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 78.9 76.9 76.5 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.5 23.4 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.179 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 260 778 N I>3s 37 37 247 778 1.0 1.0 0.7 36.3 8.9 8.9 5.3 26.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3082 Fd-3m 1 1 227 C N N N N 37 2284 0.048 3121 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.361414 8.372288 8.367937 89.9909 89.9821 90.0128 ZERR 3.00 0.000599 0.000650 0.000491 0.0055 0.0053 0.0060 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4014635- 501277 773 773 27 28.6 1216462.15 41.44 0.045 0.062 499105- 119702 1036 1036 27 38.4 213166.96 31.06 0.050 0.071 105610- 35483 862 861 27 31.9 78004.14 16.88 0.069 0.089 9985- 1835 818 813 29 28.0 3477.77 4.58 0.171 0.224 ------------------------------------------------------------------------------------------- 4014635- 1835 3489 3483 110 31.7 353475.51 23.68 0.048 0.065 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 882 878 27 32.5 635158.48 33.65 0.044 0.064 0.022 1.01-0.78 1016 1015 27 37.6 343342.99 23.90 0.037 0.047 0.027 0.78-0.65 978 978 29 33.7 231381.10 18.99 0.057 0.071 0.033 0.65-0.59 613 612 27 22.7 161278.13 16.51 0.080 0.095 0.041 ------------------------------------------------------------------------------------------------------ inf-0.59 3489 3483 110 31.7 353475.51 23.68 0.048 0.065 0.027 inf-0.60 3321 3315 99 33.5 366014.30 24.19 0.047 0.063 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 878 27 27 100.0 32.5 635158.48 214.36 0.044 0.005 1.01-0.78 1015 27 27 100.0 37.6 343342.99 157.67 0.037 0.005 0.78-0.65 978 29 29 100.0 33.7 231381.10 116.28 0.057 0.007 0.65-0.59 612 27 27 100.0 22.7 161278.13 91.31 0.080 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3483 110 110 100.0 31.7 353475.51 148.68 0.048 0.006 inf-0.60 3315 99 99 100.0 33.5 366014.30 152.76 0.047 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:01:41 2018) ID: 2932; threads 39; handles 878; mem 516864.00 (1237704.00)kB; time: 1w 5d 1h 7m 11s MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:504.8,peak PF: 697.1, WS: 295.6, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.6,peak PF: 697.1, WS: 297.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:01:41 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00060 ) 8.37691 ( 0.00065 ) 8.37554 ( 0.00049 ) 90.02113 ( 0.00553 ) 90.03240 ( 0.00533 ) 90.03043 ( 0.00605 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:01:41 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 0.000002 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007177 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000002 0.000001 0.007185 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(5) 90.021(5) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.36721(19) 8.36721(19) 8.36721(19) 90.0 90.0 90.0 V = 585.79(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb PROFFITPEAK info: 1307 peaks in the peak location table UB fit with 537 obs out of 606 (total:606,skipped:0) (88.61%) UB - matrix: -0.025241 -0.079386 -0.015669 ( 0.000024 0.000018 0.000019 ) 0.072476 -0.029375 0.032817 ( 0.000037 0.000027 0.000030 ) -0.036114 -0.003504 0.076529 ( 0.000029 0.000021 0.000023 ) M - matrix: 0.007194 0.000001 0.000010 ( 0.000006 0.000003 0.000004 ) 0.000001 0.007177 0.000012 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000012 0.007179 ( 0.000004 0.000003 0.000004 ) unit cell: 8.363(3) 8.372(2) 8.371(3) 90.09(2) 90.08(3) 90.01(2) V = 586.1(3) UB fit with 537 obs out of 606 (total:606,skipped:0) (88.61%) UB - matrix: -0.025241 -0.079386 -0.015669 ( 0.000024 0.000018 0.000019 ) 0.072476 -0.029375 0.032817 ( 0.000037 0.000027 0.000030 ) -0.036114 -0.003504 0.076529 ( 0.000029 0.000021 0.000023 ) M - matrix: 0.007194 0.000001 0.000010 ( 0.000006 0.000003 0.000004 ) 0.000001 0.007177 0.000012 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000012 0.007179 ( 0.000004 0.000003 0.000004 ) unit cell: 8.363(3) 8.372(2) 8.371(3) 90.09(2) 90.08(3) 90.01(2) V = 586.1(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: -0.025305 -0.079130 -0.015647 ( 0.000024 0.000018 0.000020 ) 0.072237 -0.029444 0.032769 ( 0.000036 0.000026 0.000029 ) -0.036065 -0.003391 0.076382 ( 0.000030 0.000022 0.000025 ) M - matrix: 0.007159 -0.000002 0.000008 ( 0.000006 0.000003 0.000004 ) -0.000002 0.007140 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000008 0.000014 0.007153 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025305 -0.079130 -0.015647 ( 0.000024 0.000018 0.000020 ) 0.072237 -0.029444 0.032769 ( 0.000036 0.000026 0.000029 ) -0.036065 -0.003391 0.076382 ( 0.000030 0.000022 0.000025 ) M - matrix: 0.007139 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007139 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007139 ( 0.000000 0.000000 0.000001 ) UB fit with 549 obs out of 606 (total:606,skipped:0) (90.59%) unit cell: 8.383(3) 8.394(2) 8.387(3) 90.11(2) 90.07(3) 89.98(2) V = 590.2(3) unit cell: 8.3880(7) 8.3880(7) 8.3880(7) 90.0 90.0 90.0 V = 590.16(9) UB fit with 549 obs out of 606 (total:606,skipped:0) (90.59%) UB - matrix: -0.025305 -0.079130 -0.015647 ( 0.000024 0.000018 0.000020 ) 0.072237 -0.029444 0.032769 ( 0.000036 0.000026 0.000029 ) -0.036065 -0.003391 0.076382 ( 0.000030 0.000022 0.000025 ) M - matrix: 0.007159 -0.000002 0.000008 ( 0.000006 0.000003 0.000004 ) -0.000002 0.007140 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000008 0.000014 0.007153 ( 0.000004 0.000003 0.000004 ) unit cell: 8.383(3) 8.394(2) 8.387(3) 90.11(2) 90.07(3) 89.98(2) V = 590.2(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 606 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.055) HKL list info: 750 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025305 -0.079130 -0.015647 ( 0.000024 0.000018 0.000020 ) 0.072237 -0.029444 0.032769 ( 0.000036 0.000026 0.000029 ) -0.036065 -0.003391 0.076382 ( 0.000030 0.000022 0.000025 ) M - matrix: 0.007159 -0.000002 0.000008 ( 0.000006 0.000003 0.000004 ) -0.000002 0.007140 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000008 0.000014 0.007153 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025305 -0.079130 -0.015647 ( 0.000024 0.000018 0.000020 ) 0.072237 -0.029444 0.032769 ( 0.000036 0.000026 0.000029 ) -0.036065 -0.003391 0.076382 ( 0.000030 0.000022 0.000025 ) M - matrix: 0.007139 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007139 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007139 ( 0.000000 0.000000 0.000001 ) UB fit with 549 obs out of 606 (total:606,skipped:0) (90.59%) unit cell: 8.383(3) 8.394(2) 8.387(3) 90.11(2) 90.07(3) 89.98(2) V = 590.2(3) unit cell: 8.3880(7) 8.3880(7) 8.3880(7) 90.0 90.0 90.0 V = 590.16(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 545 obs out of 606 (total:606,skipped:0) (89.93%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb 6 of 446 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 44 | 1.016 ( 0.150) | 1.214 ( 0.578) | 1.238 ( 1.010) | 1.41- 1.17 | 44 | 1.002 ( 0.091) | 1.108 ( 0.300) | 1.055 ( 0.552) | 1.17- 0.99 | 44 | 0.995 ( 0.090) | 1.121 ( 0.318) | 0.937 ( 0.382) | 0.99- 0.92 | 44 | 1.008 ( 0.077) | 1.040 ( 0.112) | 1.050 ( 0.424) | 0.91- 0.82 | 44 | 1.002 ( 0.077) | 1.004 ( 0.099) | 1.121 ( 0.396) | 0.82- 0.75 | 44 | 0.986 ( 0.065) | 0.975 ( 0.108) | 1.138 ( 0.440) | 0.75- 0.71 | 44 | 0.961 ( 0.052) | 0.904 ( 0.091) | 1.221 ( 0.478) | 0.71- 0.67 | 44 | 0.950 ( 0.042) | 0.880 ( 0.055) | 1.259 ( 0.448) | 0.67- 0.63 | 44 | 0.916 ( 0.044) | 0.841 ( 0.057) | 1.279 ( 0.461) | 0.63- 0.59 | 44 | 0.906 ( 0.043) | 0.823 ( 0.053) | 1.342 ( 0.534) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 440 | 0.974 ( 0.088) | 0.991 ( 0.270) | 1.164 ( 0.554) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 438 obs out of 440 (total:440,skipped:0) (99.55%) UB - matrix: -0.025297 -0.079324 -0.015487 ( 0.000014 0.000010 0.000013 ) 0.072306 -0.029433 0.032769 ( 0.000015 0.000011 0.000014 ) -0.036137 -0.003464 0.076379 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007174 0.000004 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000004 0.007171 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000001 0.007147 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3743(14) 8.3763(11) 8.3899(13) 89.995(12) 90.009(13) 90.029(12) V = 588.52(15) OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 OTKP changes: 438 1 1 1 No constraint UB - matrix: -0.025326 -0.079178 -0.015608 ( 0.000011 0.000008 0.000010 ) 0.072187 -0.029484 0.032764 ( 0.000015 0.000011 0.000014 ) -0.036075 -0.003455 0.076405 ( 0.000013 0.000009 0.000012 ) M - matrix: 0.007154 0.000002 0.000004 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007150 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000006 0.007155 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025326 -0.079178 -0.015608 ( 0.000011 0.000008 0.000010 ) 0.072187 -0.029484 0.032764 ( 0.000015 0.000011 0.000014 ) -0.036075 -0.003455 0.076405 ( 0.000013 0.000009 0.000012 ) M - matrix: 0.007150 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007150 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007150 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 440 (total:440,skipped:0) (99.77%) unit cell: 8.3861(14) 8.3881(9) 8.3855(12) 90.047(10) 90.033(12) 90.012(11) V = 589.87(14) unit cell: 8.3866(3) 8.3866(3) 8.3866(3) 90.0 90.0 90.0 V = 589.87(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.055) HKL list info: 750 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025326 -0.079178 -0.015608 ( 0.000011 0.000008 0.000010 ) 0.072187 -0.029484 0.032764 ( 0.000015 0.000011 0.000014 ) -0.036075 -0.003455 0.076405 ( 0.000013 0.000009 0.000012 ) M - matrix: 0.007154 0.000002 0.000004 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007150 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000006 0.007155 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025326 -0.079178 -0.015608 ( 0.000011 0.000008 0.000010 ) 0.072187 -0.029484 0.032764 ( 0.000015 0.000011 0.000014 ) -0.036075 -0.003455 0.076405 ( 0.000013 0.000009 0.000012 ) M - matrix: 0.007150 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007150 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007150 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 440 (total:440,skipped:0) (99.77%) unit cell: 8.3861(14) 8.3881(9) 8.3855(12) 90.047(10) 90.033(12) 90.012(11) V = 589.87(14) unit cell: 8.3866(3) 8.3866(3) 8.3866(3) 90.0 90.0 90.0 V = 589.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 440 (total:440,skipped:0) (99.77%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb 5 of 442 peaks identified as outliers and rejected 437 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 437 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 437 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.42 | 44 | 1.037 ( 0.193) | 1.240 ( 0.641) | 1.258 ( 0.981) | 1.41- 1.17 | 44 | 1.018 ( 0.101) | 1.144 ( 0.361) | 1.041 ( 0.552) | 1.17- 0.99 | 44 | 0.988 ( 0.098) | 1.073 ( 0.192) | 0.956 ( 0.400) | 0.99- 0.92 | 44 | 1.008 ( 0.078) | 1.046 ( 0.118) | 1.011 ( 0.435) | 0.91- 0.82 | 44 | 0.999 ( 0.074) | 1.006 ( 0.096) | 1.088 ( 0.397) | 0.82- 0.76 | 44 | 0.986 ( 0.065) | 0.975 ( 0.112) | 1.132 ( 0.440) | 0.76- 0.71 | 44 | 0.964 ( 0.051) | 0.905 ( 0.089) | 1.286 ( 0.514) | 0.71- 0.67 | 44 | 0.943 ( 0.039) | 0.878 ( 0.049) | 1.206 ( 0.398) | 0.67- 0.63 | 44 | 0.918 ( 0.044) | 0.848 ( 0.068) | 1.300 ( 0.483) | 0.63- 0.59 | 41 | 0.904 ( 0.045) | 0.813 ( 0.037) | 1.292 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 437 | 0.977 ( 0.099) | 0.994 ( 0.283) | 1.156 ( 0.551) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 269 | 1.115 ( 0.130) | 1.232 ( 0.467) | 1.261 ( 1.104) | 13.0-18.8 | 269 | 1.074 ( 0.052) | 1.124 ( 0.225) | 1.172 ( 0.511) | 18.8-23.0 | 269 | 1.062 ( 0.067) | 1.137 ( 0.375) | 1.152 ( 0.540) | 23.0-27.1 | 269 | 1.032 ( 0.089) | 1.072 ( 0.282) | 1.156 ( 0.561) | 27.1-30.7 | 269 | 1.006 ( 0.074) | 1.011 ( 0.254) | 1.201 ( 0.486) | 30.7-33.8 | 269 | 0.974 ( 0.076) | 0.926 ( 0.093) | 1.182 ( 0.510) | 33.8-36.9 | 269 | 0.955 ( 0.072) | 0.910 ( 0.133) | 1.146 ( 0.467) | 36.9-39.7 | 269 | 0.937 ( 0.082) | 0.867 ( 0.124) | 1.229 ( 0.556) | 39.7-42.7 | 269 | 0.919 ( 0.073) | 0.836 ( 0.079) | 1.198 ( 0.537) | 42.7-49.9 | 267 | 0.922 ( 0.083) | 0.812 ( 0.065) | 1.155 ( 0.476) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2688 | 1.000 ( 0.105) | 0.993 ( 0.281) | 1.185 ( 0.603) | Fitted profile normalization line parameters e1 dimension: a=-0.0048 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0017 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28155044 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:02:15 2018 PROFFITMAIN - Started at Tue Mar 27 16:02:15 2018 OTKP changes: 2680 2 4 6 OTKP changes: 2680 2 4 6 No constraint UB - matrix: -0.025040 -0.079515 -0.015598 ( 0.000006 0.000006 0.000006 ) 0.072519 -0.029231 0.032949 ( 0.000005 0.000006 0.000006 ) -0.036230 -0.003595 0.076552 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007199 0.000001 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007190 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000002 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025040 -0.079515 -0.015598 ( 0.000006 0.000006 0.000006 ) 0.072519 -0.029231 0.032949 ( 0.000005 0.000006 0.000006 ) -0.036230 -0.003595 0.076552 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) UB fit with 2683 obs out of 2688 (total:2688,skipped:0) (99.81%) unit cell: 8.3600(5) 8.3650(6) 8.3655(4) 90.016(5) 90.051(5) 90.012(5) V = 585.01(6) unit cell: 8.36348(14) 8.36348(14) 8.36348(14) 90.0 90.0 90.0 V = 585.006(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024874 -0.079574 -0.015663 ( 0.000013 0.000015 0.000011 ) 0.072446 -0.029203 0.032955 ( 0.000016 0.000018 0.000013 ) -0.036291 -0.003652 0.076361 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000004 0.000006 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007198 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000006 0.000005 0.007162 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3684(15) 8.3602(15) 8.3811(10) 90.041(12) 90.047(12) 89.970(14) V = 586.35(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024975 -0.079530 -0.015506 ( 0.000017 0.000014 0.000012 ) 0.072511 -0.029250 0.033016 ( 0.000012 0.000010 0.000008 ) -0.036257 -0.003634 0.076501 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000011 0.007183 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3615(11) 8.3628(14) 8.3691(11) 89.916(12) 90.060(11) 89.977(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3556(11) 8.3566(14) 8.3621(11) 89.937(12) 90.002(11) 89.958(12) V = 583.88(15) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.88(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.756) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3556(11) 8.3566(14) 8.3621(11) 89.937(12) 90.002(11) 89.958(12) V = 583.88(15) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079582 -0.015474 ( 0.000016 0.000014 0.000012 ) 0.072550 -0.029301 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003565 0.076601 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3556(11) 8.3566(14) 8.3621(11) 89.937(12) 90.002(11) 89.958(12) V = 583.88(15) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.88(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025004 -0.079545 -0.015713 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029338 0.032911 ( 0.000009 0.000014 0.000014 ) -0.036180 -0.003657 0.076519 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007179 -0.000003 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007202 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000008 0.000004 0.007185 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3715(11) 8.3583(12) 8.3678(11) 90.036(11) 90.063(11) 89.973(11) V = 585.50(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3659(10) 8.3552(12) 8.3592(11) 89.996(11) 90.020(10) 90.032(11) V = 584.29(13) unit cell: 8.3601(3) 8.3601(3) 8.3601(3) 90.0 90.0 90.0 V = 584.29(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.756) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3659(10) 8.3552(12) 8.3592(11) 89.996(11) 90.020(10) 90.032(11) V = 584.29(13) unit cell: 8.3601(3) 8.3601(3) 8.3601(3) 90.0 90.0 90.0 V = 584.29(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079565 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072396 -0.029370 0.032986 ( 0.000008 0.000014 0.000013 ) -0.036302 -0.003693 0.076581 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3659(10) 8.3552(12) 8.3592(11) 89.996(11) 90.020(10) 90.032(11) V = 584.29(13) unit cell: 8.3601(3) 8.3601(3) 8.3601(3) 90.0 90.0 90.0 V = 584.29(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025234 -0.079452 -0.015780 ( 0.000011 0.000016 0.000017 ) 0.072343 -0.029411 0.032796 ( 0.000008 0.000011 0.000012 ) -0.036275 -0.003612 0.076595 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000008 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000012 ( 0.000001 0.000003 0.000002 ) -0.000008 0.000012 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3673(10) 8.3646(14) 8.3642(11) 90.099(13) 89.938(10) 90.066(12) V = 585.40(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000000 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3594(10) 8.3604(14) 8.3563(11) 90.052(12) 89.996(10) 90.065(12) V = 584.00(14) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.00(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.756) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000000 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3594(10) 8.3604(14) 8.3563(11) 90.052(12) 89.996(10) 90.065(12) V = 584.00(14) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.00(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000000 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079493 -0.015752 ( 0.000011 0.000015 0.000017 ) 0.072468 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003658 0.076685 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3594(10) 8.3604(14) 8.3563(11) 90.052(12) 89.996(10) 90.065(12) V = 584.00(14) unit cell: 8.3587(3) 8.3587(3) 8.3587(3) 90.0 90.0 90.0 V = 584.00(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) UB - matrix: -0.025333 -0.079186 -0.015613 ( 0.000012 0.000009 0.000011 ) 0.072190 -0.029479 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036077 -0.003457 0.076406 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007155 0.000003 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007151 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000005 0.000006 0.007156 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3856(14) 8.3875(10) 8.3850(12) 90.049(11) 90.040(13) 90.021(11) V = 589.75(15) OTKP changes: 436 1 1 1 OTKP changes: 436 1 1 1 OTKP changes: 436 1 1 1 No constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007153 0.000002 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007150 0.000007 ( 0.000001 0.000002 0.000001 ) 0.000005 0.000007 0.007156 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007150 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007150 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007150 ( 0.000000 0.000000 0.000001 ) UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) unit cell: 8.3867(14) 8.3886(10) 8.3846(12) 90.053(11) 90.042(13) 90.020(11) V = 589.88(15) unit cell: 8.3866(4) 8.3866(4) 8.3866(4) 90.0 90.0 90.0 V = 589.88(4) Run 6 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.055) HKL list info: 740 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007153 0.000002 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007150 0.000007 ( 0.000001 0.000002 0.000001 ) 0.000005 0.000007 0.007156 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007150 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007150 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007150 ( 0.000000 0.000000 0.000001 ) UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) unit cell: 8.3867(14) 8.3886(10) 8.3846(12) 90.053(11) 90.042(13) 90.020(11) V = 589.88(15) unit cell: 8.3866(4) 8.3866(4) 8.3866(4) 90.0 90.0 90.0 V = 589.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007153 0.000002 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000002 0.007150 0.000007 ( 0.000001 0.000002 0.000001 ) 0.000005 0.000007 0.007156 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025335 -0.079173 -0.015624 ( 0.000012 0.000009 0.000011 ) 0.072180 -0.029483 0.032773 ( 0.000015 0.000011 0.000014 ) -0.036071 -0.003456 0.076408 ( 0.000013 0.000010 0.000012 ) M - matrix: 0.007150 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007150 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007150 ( 0.000000 0.000000 0.000001 ) UB fit with 436 obs out of 437 (total:437,skipped:0) (99.77%) unit cell: 8.3867(14) 8.3886(10) 8.3846(12) 90.053(11) 90.042(13) 90.020(11) V = 589.88(15) unit cell: 8.3866(4) 8.3866(4) 8.3866(4) 90.0 90.0 90.0 V = 589.88(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025028 -0.079382 -0.015588 ( 0.000006 0.000007 0.000007 ) 0.072492 -0.029216 0.032914 ( 0.000006 0.000007 0.000007 ) -0.036215 -0.003535 0.076497 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007193 -0.000003 0.000006 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007168 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000005 0.007178 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025028 -0.079382 -0.015588 ( 0.000006 0.000007 0.000007 ) 0.072492 -0.029216 0.032914 ( 0.000006 0.000007 0.000007 ) -0.036215 -0.003535 0.076497 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000000 ) UB fit with 2683 obs out of 2688 (total:2688,skipped:0) (99.81%) unit cell: 8.3633(6) 8.3781(7) 8.3720(5) 90.043(6) 90.046(6) 89.975(6) V = 586.61(7) unit cell: 8.3711(2) 8.3711(2) 8.3711(2) 90.0 90.0 90.0 V = 586.61(3) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region 23 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3635 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:02:23 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.756) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.756) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.756) Run 6 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.055) PROFFIT INFO: signal sum: min=255.0000 max=23148128.0000 PROFFIT INFO: signal sum lp corr: min=469.1052 max=3174806.1001 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=513 PROFFIT INFO: Inet: min=750.5683 max=5079689.5000 PROFFIT INFO: sig(Inet): min=120.3495 max=47791.3594 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.70 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 40 176 383 739 830 1505 2423 3337 3635 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.4 66.7 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3635 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3635 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5079690- 1125970 363 1877893.06 121.73 100.00 1123403- 622001 363 847126.77 102.43 100.00 621820- 265916 363 413664.05 94.70 100.00 265676- 169582 363 203129.32 71.54 100.00 169555- 119754 363 144578.86 51.08 100.00 119691- 91887 363 104758.92 35.67 100.00 91862- 65493 363 79606.74 28.95 100.00 65252- 5459 363 36989.93 19.12 100.00 5451- 2953 363 3891.95 5.28 97.25 2953- 751 368 2119.69 3.68 54.89 ------------------------------------------------------------------------------------ 5079690- 751 3635 370868.01 53.35 95.16 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 765337.62 93.97 100.00 1.41- 1.12 363 617464.95 63.42 99.45 1.12- 0.96 363 498206.21 70.35 97.52 0.96- 0.88 363 350001.41 59.83 94.49 0.88- 0.81 363 447647.61 68.58 99.45 0.81- 0.73 363 245523.87 41.17 95.59 0.73- 0.71 363 174540.82 34.22 88.71 0.71- 0.65 363 311165.27 47.48 94.21 0.65- 0.62 363 151029.03 27.16 87.60 0.62- 0.58 368 150794.63 27.69 94.57 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 370868.01 53.35 95.16 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:02:23 2018 Sorting 3635 observations 120 unique observations with > 7.00 F2/sig(F2) 3635 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 99 621 Total number of frames 621 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3635 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 16 106 Total number of frames 106 2920 observations > 7.00 F2/sig(F2) 2920 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 16 106 Total number of frames 106 Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2920 removed 3 = 2917, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2917 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 16 106 Total number of frames 106 130 unique data precomputed (should be 130) 130 unique data with 2917 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.4 (Out of 2917 removed 0 = 2917, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 2917 observations RMS deviation of equivalent data = 0.25098 Rint = 0.18126 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17441, wR= 0.25634 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13176, wR= 0.16928, Acormin=0.613, Acormax=1.406, Acor_av=0.996 F test: Probability=1.000, F= 1.749 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11892, wR= 0.14830, Acormin=0.551, Acormax=1.444, Acor_av=0.912 F test: Probability=1.000, F= 1.226 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10597, wR= 0.14088, Acormin=0.656, Acormax=1.617, Acor_av=0.984 F test: Probability=1.000, F= 1.257 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09189, wR= 0.12138, Acormin=0.537, Acormax=1.563, Acor_av=0.899 F test: Probability=1.000, F= 1.328 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08017, wR= 0.10952, Acormin=0.512, Acormax=1.629, Acor_av=0.913 F test: Probability=1.000, F= 1.311 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09790, wR= 0.13352, Acormin=0.649, Acormax=1.693, Acor_av=0.989 F test: Probability=0.000, F= 0.670 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08564, wR= 0.11530, Acormin=0.519, Acormax=1.637, Acor_av=0.908 F test: Probability=0.000, F= 0.874 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07609, wR= 0.10577, Acormin=0.500, Acormax=1.661, Acor_av=0.918 F test: Probability=0.996, F= 1.105 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07310, wR= 0.10043, Acormin=0.388, Acormax=1.546, Acor_av=0.873 F test: Probability=0.977, F= 1.079 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09954, wR= 0.12996, Acormin=0.498, Acormax=1.499, Acor_av=0.856 F test: Probability=0.000, F= 0.540 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08427, wR= 0.11127, Acormin=0.511, Acormax=1.634, Acor_av=0.897 F test: Probability=0.000, F= 0.753 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08255, wR= 0.10872, Acormin=0.119, Acormax=0.428, Acor_av=0.233 F test: Probability=0.000, F= 0.782 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07555, wR= 0.10107, Acormin=0.117, Acormax=0.447, Acor_av=0.255 F test: Probability=0.000, F= 0.930 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07072, wR= 0.09533, Acormin=0.127, Acormax=0.463, Acor_av=0.263 F test: Probability=0.921, F= 1.056 Final absorption model (ne=6, no=5): Rint= 0.07310, Acormin=0.388, Acormax=1.546, Acor_av=0.873 Combined refinement in use Rint: 0.18137 There are 106 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 153 pars with 11781 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25098 Using Levenberg-Marquardt: 0.00010 New wR= 0.06336 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18126 with corrections 0.05024 Rint for all data: 0.18137 with corrections 0.05047 0 observations identified as outliers and rejected Cycle 2 wR= 0.06336 Using Levenberg-Marquardt: 0.00001 New wR= 0.06043 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18126 with corrections 0.04747 Rint for all data: 0.18137 with corrections 0.04769 0 observations identified as outliers and rejected Cycle 3 wR= 0.06043 Using Levenberg-Marquardt: 0.00000 New wR= 0.05987 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18126 with corrections 0.04692 Rint for all data: 0.18137 with corrections 0.04714 0 observations identified as outliers and rejected Cycle 4 wR= 0.05987 Using Levenberg-Marquardt: 0.00000 New wR= 0.05958 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18126 with corrections 0.04665 Rint for all data: 0.18137 with corrections 0.04687 0 observations identified as outliers and rejected Cycle 5 wR= 0.05958 Using Levenberg-Marquardt: 0.00000 New wR= 0.05941 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18126 with corrections 0.04649 Rint for all data: 0.18137 with corrections 0.04671 0 observations identified as outliers and rejected Final wR= 0.05941 Final frame scales: Min= 0.7442 Max= 1.3041 Final absorption correction factors: Amin= 0.4840 Amax= 1.3790 PROFFIT INFO: Inet (after scale3 abspack): min=747.2324 max=4599403.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=143.8345 max=53497.3320 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3635 reflections read from tmp file 775 reflections are rejected (775 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 2 2 7 1 5 4 2 128 Initial Chi^2= 0.42715 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93008 Current error model SIG(F2)^2 = 157.30*I_RAW + 0.00*I_BACK+(0.01608*)^2 Cycle 2, Chi^2= 1.01260 Current error model SIG(F2)^2 = 107.12*I_RAW + 0.00*I_BACK+(0.02233*)^2 Cycle 3, Chi^2= 1.00055 Current error model SIG(F2)^2 = 116.50*I_RAW + 0.00*I_BACK+(0.02061*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 115.49*I_RAW + 0.00*I_BACK+(0.02085*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 115.66*I_RAW + 0.00*I_BACK+(0.02081*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 115.66*I_RAW + 0.00*I_BACK+(0.02081*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4599403- 1094242 363 1778862.83 44.78 100.00 1092756- 601855 363 808546.48 37.63 100.00 601688- 256656 363 402467.80 36.14 100.00 256217- 154003 363 192777.39 31.73 100.00 153895- 124392 363 139314.19 25.65 100.00 124303- 86928 363 101269.69 19.63 100.00 86895- 68034 363 77764.15 16.88 100.00 67962- 4862 363 39058.63 12.06 100.00 4849- 2748 363 3602.64 4.63 96.42 2738- 747 368 2132.14 3.78 75.00 ------------------------------------------------------------------------------------ 4599403- 747 3635 354094.80 23.26 97.11 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 767072.27 36.80 100.00 1.41- 1.12 363 597820.11 28.82 99.45 1.12- 0.96 363 459308.60 27.68 98.62 0.96- 0.88 363 330250.48 23.86 97.25 0.88- 0.81 363 423368.59 27.32 99.72 0.81- 0.73 363 225797.93 18.90 96.69 0.73- 0.71 363 166334.18 17.46 92.01 0.71- 0.65 363 292393.59 22.38 98.07 0.65- 0.62 363 141682.62 14.51 92.29 0.62- 0.58 368 139870.35 15.05 97.01 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 354094.80 23.26 97.11 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 767072.27 36.80 100.00 4.82- 1.12 726 682446.19 32.81 99.72 4.82- 0.96 1089 608066.99 31.10 99.36 4.82- 0.88 1452 538612.86 29.29 98.83 4.82- 0.81 1815 515564.01 28.89 99.01 4.82- 0.73 2178 467269.66 27.23 98.62 4.82- 0.71 2541 424278.88 25.83 97.68 4.82- 0.65 2904 407793.22 25.40 97.73 4.82- 0.62 3267 378225.37 24.19 97.12 4.82- 0.58 3635 354094.80 23.26 97.11 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 354094.80 23.26 97.11 Scale applied to data: s=0.217419 (maximum obs:4599403.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.028: data 3635 -> merged 157 With outlier rejection... Rint 0.046; Rsigma 0.028: data 3624 -> merged 157 Rejected total: 11, method kkm 8, method Blessing 3 Completeness direct cell (a, b, c) = (8.371, 8.371, 8.371), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586095, 4.833061 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.48 14 14 21.14 100.00 296 1.41 - 1.12 14 14 29.86 100.00 418 1.12 - 0.97 14 14 29.64 100.00 415 0.96 - 0.84 14 14 31.93 100.00 447 0.84 - 0.78 14 14 24.29 100.00 340 0.78 - 0.73 14 14 25.71 100.00 360 0.73 - 0.69 14 14 23.50 100.00 329 0.69 - 0.66 14 14 20.71 100.00 290 0.65 - 0.63 14 14 21.07 100.00 295 0.63 - 0.60 14 14 18.79 100.00 263 --------------------------------------------------------------- 8.39 - 0.60 140 140 24.66 100.00 3453 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:02:24 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.363286 8.378074 8.371973 90.0429 90.0459 89.9747 3624 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.28 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1852 0 2434 2434 3624 N (int>3sigma) = 0 0 0 0 1852 0 2363 2358 3519 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.5 79.4 77.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.61 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 Unitcell: 5.914 5.918 5.919 119.93 90.06 119.96 Niggli form: a.a = 34.981 b.b = 35.019 c.c = 35.037 b.c = -17.479 a.c = -0.036 a.b = -17.478 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.054 CUBIC F-lattice R(int) = 0.046 [ 3467] Vol = 586.6 Cell: 8.363 8.378 8.372 90.04 89.95 90.03 Volume: 586.61 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.051 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 3185] Vol = 440.0 Cell: 5.918 5.914 14.509 89.94 90.08 119.96 Volume: 439.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 -0.5000 1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.051 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1021] Vol = 440.0 Trigonal Cell: 5.918 5.914 14.509 89.94 90.08 119.96 Volume: 439.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 -0.5000 1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.082 TETRAGONAL I-lattice R(int) = 0.045 [ 3217] Vol = 293.3 Cell: 5.920 5.924 8.363 89.95 89.99 90.04 Volume: 293.30 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.081 TETRAGONAL I-lattice R(int) = 0.045 [ 3217] Vol = 293.3 Cell: 5.920 5.924 8.363 89.95 89.99 90.04 Volume: 293.30 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.073 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3161] Vol = 293.3 Cell: 5.920 8.363 5.924 89.95 89.96 90.01 Volume: 293.30 Matrix: 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.039 MONOCLINIC I-lattice R(int) = 0.045 [ 2811] Vol = 293.3 Cell: 8.363 5.920 5.924 90.04 90.05 90.01 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.039 MONOCLINIC I-lattice R(int) = 0.043 [ 2814] Vol = 293.3 Cell: 5.919 5.914 8.378 90.01 90.05 89.94 Volume: 293.30 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.037 MONOCLINIC C-lattice R(int) = 0.043 [ 2825] Vol = 293.3 Cell: 8.363 8.378 5.914 90.01 134.95 90.03 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2139] Vol = 146.7 Cell: 5.914 5.918 5.919 119.93 90.06 119.96 Volume: 146.65 Matrix:-0.5000 0.0000 -0.5000 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1852 0 2445 2428 3624 N (int>3sigma) = 0 0 0 0 1852 0 2374 2355 3519 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.6 77.1 77.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.3 23.3 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.147 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 271 809 N I>3s 38 38 258 809 1.0 1.0 0.7 36.3 8.9 8.9 5.4 26.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.046 3216 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3255 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363286 8.378074 8.371973 90.0429 89.9541 90.0253 ZERR 3.00 0.000626 0.000663 0.000519 0.0057 0.0056 0.0062 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 4001867- 744568 591 590 26 22.7 1434934.44 42.48 0.041 0.055 734818- 224550 567 566 26 21.8 447851.71 36.22 0.061 0.079 219848- 96248 839 839 26 32.3 148087.43 26.35 0.043 0.056 93816- 69484 583 581 26 22.3 81745.17 17.09 0.069 0.087 64998- 3572 472 469 26 18.0 26081.45 9.18 0.084 0.109 3401- 1717 583 579 27 21.4 2643.51 4.24 0.196 0.254 ------------------------------------------------------------------------------------------- 4001867- 1717 3635 3624 157 23.1 354745.44 23.28 0.046 0.062 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 678 673 26 25.9 624009.94 32.07 0.047 0.063 0.023 1.12-0.88 803 801 26 30.8 457776.25 27.04 0.034 0.046 0.025 0.85-0.75 675 675 26 26.0 324010.70 22.65 0.042 0.052 0.029 0.74-0.68 590 589 26 22.7 254687.80 20.37 0.057 0.069 0.033 0.67-0.63 559 559 26 21.5 146642.89 16.04 0.076 0.092 0.042 0.62-0.59 330 327 27 12.1 147609.47 14.92 0.073 0.084 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3635 3624 157 23.1 354745.44 23.28 0.046 0.062 0.028 inf-0.60 3460 3451 139 24.8 367055.90 23.76 0.046 0.061 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 673 26 26 100.0 25.9 624009.94 177.34 0.047 0.006 1.12-0.88 801 26 26 100.0 30.8 457776.25 152.70 0.034 0.005 0.85-0.75 675 26 26 100.0 26.0 324010.70 121.94 0.042 0.006 0.74-0.68 589 26 26 100.0 22.7 254687.80 98.87 0.057 0.008 0.67-0.63 559 26 26 100.0 21.5 146642.89 73.72 0.076 0.009 0.62-0.59 327 27 27 100.0 12.1 147609.47 60.08 0.073 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3624 157 157 100.0 23.1 354745.44 122.26 0.046 0.007 inf-0.60 3451 139 139 100.0 24.8 367055.90 125.90 0.046 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025028 -0.079381 -0.015587 ( 0.000006 0.000007 0.000007 ) 0.072492 -0.029216 0.032914 ( 0.000007 0.000007 0.000007 ) -0.036215 -0.003535 0.076497 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007193 -0.000003 0.000006 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007167 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000005 0.007178 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025028 -0.079381 -0.015587 ( 0.000006 0.000007 0.000007 ) 0.072492 -0.029216 0.032914 ( 0.000007 0.000007 0.000007 ) -0.036215 -0.003535 0.076497 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3633(6) 8.3781(7) 8.3720(5) 90.043(6) 90.046(6) 89.974(6) V = 586.61(7) unit cell: 8.3711(2) 8.3711(2) 8.3711(2) 90.0 90.0 90.0 V = 586.61(3) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.756) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.756) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.756) Run 6 Omega scan: (-1.000 - 99.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=53.055) PROFFIT INFO: signal sum: min=255.0000 max=23148128.0000 PROFFIT INFO: signal sum lp corr: min=469.1052 max=3174806.1001 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=513 PROFFIT INFO: Inet: min=750.5683 max=5079689.5000 PROFFIT INFO: sig(Inet): min=120.3495 max=47791.3594 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.70 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 80 352 766 1478 1660 3010 4846 6674 7270 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.8 41.4 66.7 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3635 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3635 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5079690- 1125970 363 1877893.06 121.73 100.00 1123403- 622001 363 847126.77 102.43 100.00 621820- 265916 363 413664.05 94.70 100.00 265676- 169582 363 203129.32 71.54 100.00 169555- 119754 363 144578.86 51.08 100.00 119691- 91887 363 104758.92 35.67 100.00 91862- 65493 363 79606.74 28.95 100.00 65252- 5459 363 36989.93 19.12 100.00 5451- 2953 363 3891.95 5.28 97.25 2953- 751 368 2119.69 3.68 54.89 ------------------------------------------------------------------------------------ 5079690- 751 3635 370868.01 53.35 95.16 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 765337.62 93.97 100.00 1.41- 1.12 363 617464.95 63.42 99.45 1.12- 0.96 363 498206.21 70.35 97.52 0.96- 0.88 363 350001.41 59.83 94.49 0.88- 0.81 363 447647.61 68.58 99.45 0.81- 0.73 363 245523.87 41.17 95.59 0.73- 0.71 363 174540.82 34.22 88.71 0.71- 0.65 363 311165.27 47.48 94.21 0.65- 0.62 363 151029.03 27.16 87.60 0.62- 0.58 368 150794.63 27.69 94.57 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 370868.01 53.35 95.16 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:02:25 2018 Sorting 3635 observations 86 unique observations with > 7.00 F2/sig(F2) 3635 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 99 621 Total number of frames 621 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3635 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 12 81 Total number of frames 81 2920 observations > 7.00 F2/sig(F2) 2920 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 12 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 31.4 (Out of 2920 removed 3 = 2917, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2917 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 12 81 Total number of frames 81 93 unique data precomputed (should be 93) 93 unique data with 2917 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 31.4 (Out of 2917 removed 0 = 2917, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2917 observations RMS deviation of equivalent data = 0.25137 Rint = 0.18151 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17460, wR= 0.25672 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13186, wR= 0.16972, Acormin=0.612, Acormax=1.406, Acor_av=0.996 F test: Probability=1.000, F= 1.750 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11936, wR= 0.14882, Acormin=0.551, Acormax=1.444, Acor_av=0.912 F test: Probability=1.000, F= 1.219 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10618, wR= 0.14136, Acormin=0.657, Acormax=1.618, Acor_av=0.985 F test: Probability=1.000, F= 1.261 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09213, wR= 0.12192, Acormin=0.536, Acormax=1.562, Acor_av=0.899 F test: Probability=1.000, F= 1.327 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08027, wR= 0.11000, Acormin=0.511, Acormax=1.628, Acor_av=0.913 F test: Probability=1.000, F= 1.314 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09768, wR= 0.13375, Acormin=0.650, Acormax=1.699, Acor_av=0.991 F test: Probability=0.000, F= 0.675 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08573, wR= 0.11556, Acormin=0.520, Acormax=1.639, Acor_av=0.909 F test: Probability=0.000, F= 0.875 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07616, wR= 0.10600, Acormin=0.502, Acormax=1.665, Acor_av=0.919 F test: Probability=0.996, F= 1.106 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07327, wR= 0.10075, Acormin=0.393, Acormax=1.550, Acor_av=0.875 F test: Probability=0.973, F= 1.076 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09961, wR= 0.13038, Acormin=0.508, Acormax=1.506, Acor_av=0.858 F test: Probability=0.000, F= 0.542 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08413, wR= 0.11150, Acormin=0.514, Acormax=1.641, Acor_av=0.898 F test: Probability=0.000, F= 0.759 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08266, wR= 0.10924, Acormin=0.118, Acormax=0.425, Acor_av=0.231 F test: Probability=0.000, F= 0.784 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07571, wR= 0.10171, Acormin=0.118, Acormax=0.443, Acor_av=0.252 F test: Probability=0.000, F= 0.931 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07102, wR= 0.09588, Acormin=0.125, Acormax=0.459, Acor_av=0.260 F test: Probability=0.908, F= 1.052 Final absorption model (ne=6, no=5): Rint= 0.07327, Acormin=0.393, Acormax=1.550, Acor_av=0.875 Combined refinement in use Rint: 0.18162 There are 81 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25137 Using Levenberg-Marquardt: 0.00010 New wR= 0.06537 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18151 with corrections 0.05126 Rint for all data: 0.18162 with corrections 0.05148 0 observations identified as outliers and rejected Cycle 2 wR= 0.06537 Using Levenberg-Marquardt: 0.00001 New wR= 0.06242 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18151 with corrections 0.04888 Rint for all data: 0.18162 with corrections 0.04910 0 observations identified as outliers and rejected Cycle 3 wR= 0.06242 Using Levenberg-Marquardt: 0.00000 New wR= 0.06171 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18151 with corrections 0.04834 Rint for all data: 0.18162 with corrections 0.04856 0 observations identified as outliers and rejected Cycle 4 wR= 0.06171 Using Levenberg-Marquardt: 0.00000 New wR= 0.06137 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18151 with corrections 0.04809 Rint for all data: 0.18162 with corrections 0.04831 0 observations identified as outliers and rejected Cycle 5 wR= 0.06137 Using Levenberg-Marquardt: 0.00000 New wR= 0.06115 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18151 with corrections 0.04795 Rint for all data: 0.18162 with corrections 0.04817 0 observations identified as outliers and rejected Final wR= 0.06115 Final frame scales: Min= 0.8049 Max= 1.3301 Final absorption correction factors: Amin= 0.4939 Amax= 1.4108 PROFFIT INFO: Inet (after scale3 abspack): min=750.3378 max=4697676.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=142.1177 max=53297.0273 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3635 reflections read from tmp file 786 reflections are rejected (786 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 3 2 5 1 2 2 4 89 Initial Chi^2= 0.41740 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.22826 Current error model SIG(F2)^2 = 171.41*I_RAW + 0.00*I_BACK+(0.01027*)^2 Cycle 2, Chi^2= 1.16037 Current error model SIG(F2)^2 = 76.01*I_RAW + 0.00*I_BACK+(0.02652*)^2 Cycle 3, Chi^2= 1.00115 Current error model SIG(F2)^2 = 116.14*I_RAW + 0.00*I_BACK+(0.02161*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 114.64*I_RAW + 0.00*I_BACK+(0.02195*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 114.94*I_RAW + 0.00*I_BACK+(0.02188*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 114.94*I_RAW + 0.00*I_BACK+(0.02188*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4697677- 1091571 363 1776546.81 42.90 100.00 1090199- 600824 363 808918.66 36.53 100.00 600404- 257497 363 402292.84 35.08 100.00 256983- 153508 363 192569.50 31.03 100.00 153454- 124480 363 139416.13 25.26 100.00 124427- 86854 363 101337.78 19.55 100.00 86745- 68114 363 77700.26 16.79 100.00 67909- 4902 363 39090.34 12.02 100.00 4894- 2745 363 3603.49 4.66 96.42 2744- 750 368 2131.14 3.79 75.54 ------------------------------------------------------------------------------------ 4697677- 750 3635 353876.20 22.73 97.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 764750.00 35.48 100.00 1.41- 1.12 363 597591.62 27.93 99.45 1.12- 0.96 363 459204.06 26.95 98.62 0.96- 0.88 363 330433.86 23.33 97.25 0.88- 0.81 363 423271.68 26.69 99.72 0.81- 0.73 363 225914.59 18.57 96.69 0.73- 0.71 363 166502.76 17.25 92.29 0.71- 0.65 363 292171.60 22.01 98.07 0.65- 0.62 363 141697.19 14.35 92.29 0.62- 0.58 368 140168.25 14.91 97.28 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 353876.20 22.73 97.17 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 363 764750.00 35.48 100.00 4.82- 1.12 726 681170.81 31.70 99.72 4.82- 0.96 1089 607181.89 30.12 99.36 4.82- 0.88 1452 537994.88 28.42 98.83 4.82- 0.81 1815 515050.24 28.07 99.01 4.82- 0.73 2178 466860.97 26.49 98.62 4.82- 0.71 2541 423952.65 25.17 97.72 4.82- 0.65 2904 407480.02 24.77 97.76 4.82- 0.62 3267 377948.59 23.62 97.15 4.82- 0.58 3635 353876.20 22.73 97.17 ------------------------------------------------------------------------------------ 4.82- 0.58 3635 353876.20 22.73 97.17 Scale applied to data: s=0.212871 (maximum obs:4697676.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.029: data 3635 -> merged 110 With outlier rejection... Rint 0.048; Rsigma 0.029: data 3624 -> merged 110 Rejected total: 11, method kkm 8, method Blessing 3 Completeness direct cell (a, b, c) = (8.371, 8.371, 8.371), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.586096, 4.833075 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.39 - 1.71 10 10 22.50 100.00 225 1.61 - 1.21 10 10 33.40 100.00 334 1.17 - 1.02 10 10 43.00 100.00 430 0.99 - 0.89 10 10 42.00 100.00 420 0.88 - 0.81 10 10 40.30 100.00 403 0.81 - 0.74 10 10 35.20 100.00 352 0.73 - 0.71 10 10 38.10 100.00 381 0.70 - 0.66 10 10 32.60 100.00 326 0.66 - 0.64 10 10 29.50 100.00 295 0.63 - 0.60 10 10 28.60 100.00 286 --------------------------------------------------------------- 8.39 - 0.60 100 100 34.52 100.00 3452 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:02:24 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.363286 8.378074 8.371973 90.0429 90.0459 89.9747 3624 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.28 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1852 0 2434 2434 3624 N (int>3sigma) = 0 0 0 0 1852 0 2363 2358 3519 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.5 79.4 77.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.61 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.0000 -0.5000 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 Unitcell: 5.914 5.918 5.919 119.93 90.06 119.96 Niggli form: a.a = 34.981 b.b = 35.019 c.c = 35.037 b.c = -17.479 a.c = -0.036 a.b = -17.478 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.054 CUBIC F-lattice R(int) = 0.046 [ 3467] Vol = 586.6 Cell: 8.363 8.378 8.372 90.04 89.95 90.03 Volume: 586.61 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.051 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 3185] Vol = 440.0 Cell: 5.918 5.914 14.509 89.94 90.08 119.96 Volume: 439.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 -0.5000 1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.051 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1021] Vol = 440.0 Trigonal Cell: 5.918 5.914 14.509 89.94 90.08 119.96 Volume: 439.96 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 -0.5000 1.0000 1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.082 TETRAGONAL I-lattice R(int) = 0.045 [ 3217] Vol = 293.3 Cell: 5.920 5.924 8.363 89.95 89.99 90.04 Volume: 293.30 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.081 TETRAGONAL I-lattice R(int) = 0.045 [ 3217] Vol = 293.3 Cell: 5.920 5.924 8.363 89.95 89.99 90.04 Volume: 293.30 Matrix: 0.0000 -0.5000 -0.5000 0.0000 0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.073 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3161] Vol = 293.3 Cell: 5.920 8.363 5.924 89.95 89.96 90.01 Volume: 293.30 Matrix: 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.039 MONOCLINIC I-lattice R(int) = 0.045 [ 2811] Vol = 293.3 Cell: 8.363 5.920 5.924 90.04 90.05 90.01 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.039 MONOCLINIC I-lattice R(int) = 0.043 [ 2814] Vol = 293.3 Cell: 5.919 5.914 8.378 90.01 90.05 89.94 Volume: 293.30 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.037 MONOCLINIC C-lattice R(int) = 0.043 [ 2825] Vol = 293.3 Cell: 8.363 8.378 5.914 90.01 134.95 90.03 Volume: 293.30 Matrix: 1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2139] Vol = 146.7 Cell: 5.914 5.918 5.919 119.93 90.06 119.96 Volume: 146.65 Matrix:-0.5000 0.0000 -0.5000 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1852 0 2445 2428 3624 N (int>3sigma) = 0 0 0 0 1852 0 2374 2355 3519 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.6 77.1 77.1 Mean int/sigma = 0.0 0.0 0.0 0.0 24.1 0.0 23.3 23.3 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.147 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 271 809 N I>3s 38 38 258 809 1.0 1.0 0.7 36.3 8.9 8.9 5.4 26.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.046 3216 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3255 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363286 8.378074 8.371973 90.0429 89.9541 90.0253 ZERR 3.00 0.000626 0.000663 0.000519 0.0057 0.0056 0.0062 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3988637- 508264 803 802 27 29.7 1222731.44 38.96 0.045 0.063 503865- 119613 1083 1083 27 40.1 214213.35 29.89 0.051 0.067 105601- 35471 896 894 27 33.1 77848.16 16.76 0.069 0.088 10362- 1848 853 845 29 29.1 3451.66 4.58 0.167 0.210 ------------------------------------------------------------------------------------------- 3988637- 1848 3635 3624 110 32.9 354618.26 22.75 0.048 0.065 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 918 913 27 33.8 641560.71 31.80 0.045 0.065 0.024 1.02-0.78 1089 1087 27 40.3 332830.68 22.42 0.038 0.047 0.029 0.78-0.65 966 965 28 34.5 243608.11 19.33 0.057 0.071 0.034 0.65-0.59 662 659 28 23.5 155573.40 15.79 0.079 0.098 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3635 3624 110 32.9 354618.26 22.75 0.048 0.065 0.029 inf-0.60 3460 3450 99 34.8 366876.25 23.21 0.047 0.064 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 913 27 27 100.0 33.8 641560.71 207.57 0.045 0.006 1.02-0.78 1087 27 27 100.0 40.3 332830.68 151.63 0.038 0.005 0.78-0.65 965 28 28 100.0 34.5 243608.11 120.71 0.057 0.007 0.65-0.59 659 28 28 100.0 23.5 155573.40 88.20 0.079 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3624 110 110 100.0 32.9 354618.26 145.95 0.048 0.006 inf-0.60 3450 99 99 100.0 34.8 366876.25 149.81 0.047 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:04:35 2018) ID: 2932; threads 38; handles 877; mem 517200.00 (1229512.00)kB; time: 1w 5d 1h 10m 6s MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1200.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:505.1,peak PF: 697.1, WS: 295.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:227.0, V:1202.0; MEMORY INFO: Process info - Handles: 878, Memory: PF:506.9,peak PF: 697.1, WS: 297.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:04:35 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000007 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000005 0.000005 0.000005 ) 8.37024 ( 0.00063 ) 8.37691 ( 0.00066 ) 8.37554 ( 0.00052 ) 90.02113 ( 0.00573 ) 90.03240 ( 0.00560 ) 90.03043 ( 0.00622 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:04:36 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000007 0.000007 ) 0.072431 -0.029136 0.032908 ( 0.000007 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000005 0.000005 0.000005 ) M - matrix: 0.007193 -0.000003 0.000006 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007167 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000005 0.007178 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(7) 8.3755(5) 90.021(6) 90.032(6) 90.030(6) V = 587.27(7) unit cell: 8.3711(2) 8.3711(2) 8.3711(2) 90.0 90.0 90.0 V = 586.61(3) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb PROFFITPEAK info: 1407 peaks in the peak location table UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 650 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) unit cell: 8.3672(7) 8.3672(7) 8.3672(7) 90.0 90.0 90.0 V = 585.79(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 272 | 1.116 ( 0.128) | 1.237 ( 0.470) | 1.268 ( 1.090) | 12.9-18.7 | 272 | 1.076 ( 0.052) | 1.125 ( 0.224) | 1.166 ( 0.510) | 18.7-22.9 | 272 | 1.062 ( 0.067) | 1.135 ( 0.373) | 1.156 ( 0.539) | 22.9-27.1 | 272 | 1.032 ( 0.088) | 1.075 ( 0.285) | 1.140 ( 0.552) | 27.1-30.6 | 272 | 1.007 ( 0.073) | 1.014 ( 0.265) | 1.202 ( 0.490) | 30.6-33.8 | 272 | 0.974 ( 0.076) | 0.927 ( 0.092) | 1.181 ( 0.513) | 33.8-36.9 | 273 | 0.956 ( 0.071) | 0.905 ( 0.116) | 1.150 ( 0.463) | 36.9-39.7 | 272 | 0.938 ( 0.081) | 0.869 ( 0.124) | 1.222 ( 0.549) | 39.7-42.7 | 272 | 0.919 ( 0.074) | 0.839 ( 0.090) | 1.192 ( 0.542) | 42.7-49.9 | 275 | 0.922 ( 0.082) | 0.813 ( 0.068) | 1.166 ( 0.480) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-49.9 | 2724 | 1.000 ( 0.105) | 0.994 ( 0.283) | 1.184 ( 0.600) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0016 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:05:10 2018 PROFFITMAIN - Started at Tue Mar 27 16:05:10 2018 OTKP changes: 2716 2 4 6 OTKP changes: 2716 2 4 6 No constraint UB - matrix: -0.025044 -0.079511 -0.015600 ( 0.000006 0.000006 0.000006 ) 0.072519 -0.029233 0.032947 ( 0.000005 0.000005 0.000005 ) -0.036229 -0.003596 0.076552 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007199 0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) 0.000002 0.007189 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000007 0.000002 0.007189 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025044 -0.079511 -0.015600 ( 0.000006 0.000006 0.000006 ) 0.072519 -0.029233 0.032947 ( 0.000005 0.000005 0.000005 ) -0.036229 -0.003596 0.076552 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) UB fit with 2719 obs out of 2724 (total:2724,skipped:0) (99.82%) unit cell: 8.3599(5) 8.3653(6) 8.3655(4) 90.015(5) 90.053(5) 90.013(5) V = 585.03(6) unit cell: 8.36359(14) 8.36359(14) 8.36359(14) 90.0 90.0 90.0 V = 585.030(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024874 -0.079572 -0.015663 ( 0.000013 0.000015 0.000011 ) 0.072446 -0.029206 0.032955 ( 0.000016 0.000018 0.000013 ) -0.036291 -0.003653 0.076361 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000004 0.000006 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007198 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000006 0.000005 0.007162 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3683(15) 8.3603(15) 8.3811(10) 90.039(12) 90.047(12) 89.968(14) V = 586.36(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007177 -0.000005 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3726(14) 8.3674(14) 8.3778(10) 89.995(11) 89.976(12) 89.964(14) V = 586.92(16) unit cell: 8.3726(3) 8.3726(3) 8.3726(3) 90.0 90.0 90.0 V = 586.92(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.918) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007177 -0.000005 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3726(14) 8.3674(14) 8.3778(10) 89.995(11) 89.976(12) 89.964(14) V = 586.92(16) unit cell: 8.3726(3) 8.3726(3) 8.3726(3) 90.0 90.0 90.0 V = 586.92(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007177 -0.000005 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024799 -0.079523 -0.015573 ( 0.000012 0.000014 0.000010 ) 0.072439 -0.029128 0.032888 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076445 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3726(14) 8.3674(14) 8.3778(10) 89.995(11) 89.976(12) 89.964(14) V = 586.92(16) unit cell: 8.3726(3) 8.3726(3) 8.3726(3) 90.0 90.0 90.0 V = 586.92(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024975 -0.079530 -0.015506 ( 0.000017 0.000014 0.000012 ) 0.072511 -0.029250 0.033016 ( 0.000012 0.000010 0.000008 ) -0.036257 -0.003635 0.076501 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000008 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000008 -0.000011 0.007183 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3614(11) 8.3628(14) 8.3691(11) 89.916(12) 90.061(11) 89.977(12) V = 585.21(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3567(14) 8.3622(11) 89.937(12) 90.002(11) 89.958(12) V = 583.90(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3567(14) 8.3622(11) 89.937(12) 90.002(11) 89.958(12) V = 583.90(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007206 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007204 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007195 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025019 -0.079580 -0.015475 ( 0.000016 0.000014 0.000012 ) 0.072549 -0.029300 0.032981 ( 0.000011 0.000010 0.000008 ) -0.036288 -0.003566 0.076600 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3557(11) 8.3567(14) 8.3622(11) 89.937(12) 90.002(11) 89.958(12) V = 583.90(15) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025004 -0.079545 -0.015713 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029338 0.032911 ( 0.000009 0.000014 0.000014 ) -0.036180 -0.003657 0.076519 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007179 -0.000003 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007202 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000008 0.000004 0.007185 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3715(11) 8.3583(12) 8.3678(11) 90.036(11) 90.063(11) 89.973(11) V = 585.50(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3593(11) 89.996(11) 90.020(10) 90.031(11) V = 584.32(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.32(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3593(11) 89.996(11) 90.020(10) 90.031(11) V = 584.32(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.32(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007188 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007207 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007200 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025088 -0.079564 -0.015724 ( 0.000008 0.000013 0.000013 ) 0.072395 -0.029370 0.032985 ( 0.000008 0.000014 0.000013 ) -0.036301 -0.003693 0.076580 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3660(10) 8.3553(12) 8.3593(11) 89.996(11) 90.020(10) 90.031(11) V = 584.32(13) unit cell: 8.3602(3) 8.3602(3) 8.3602(3) 90.0 90.0 90.0 V = 584.32(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025234 -0.079452 -0.015780 ( 0.000011 0.000016 0.000017 ) 0.072343 -0.029411 0.032797 ( 0.000008 0.000011 0.000012 ) -0.036276 -0.003612 0.076595 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000008 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000012 ( 0.000001 0.000003 0.000002 ) -0.000008 0.000012 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3673(10) 8.3646(14) 8.3642(11) 90.100(13) 89.938(10) 90.066(12) V = 585.40(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.02(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.02(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007198 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025257 -0.079491 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072466 -0.029420 0.032806 ( 0.000008 0.000011 0.000012 ) -0.036196 -0.003657 0.076684 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3595(10) 8.3605(14) 8.3564(11) 90.052(12) 89.996(10) 90.065(11) V = 584.02(14) unit cell: 8.3588(3) 8.3588(3) 8.3588(3) 90.0 90.0 90.0 V = 584.02(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 791 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) unit cell: 8.3674(3) 8.3674(3) 8.3674(3) 90.0 90.0 90.0 V = 585.82(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) unit cell: 8.3674(3) 8.3674(3) 8.3674(3) 90.0 90.0 90.0 V = 585.82(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025035 -0.079418 -0.015578 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029214 0.032909 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003579 0.076537 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000000 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007174 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000002 0.007184 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025035 -0.079418 -0.015578 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029214 0.032909 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003579 0.076537 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2719 obs out of 2724 (total:2724,skipped:0) (99.82%) unit cell: 8.3613(6) 8.3746(6) 8.3687(5) 90.015(5) 90.032(5) 89.997(6) V = 586.00(7) unit cell: 8.36820(18) 8.36820(18) 8.36820(18) 90.0 90.0 90.0 V = 586.00(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 72 reflections under beam stop or inside a detector rejection region 23 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof 3684 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:05:19 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.918) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) PROFFIT INFO: signal sum: min=255.0000 max=23168420.0000 PROFFIT INFO: signal sum lp corr: min=468.6985 max=3209345.9464 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=501 PROFFIT INFO: Inet: min=749.9176 max=5134953.5000 PROFFIT INFO: sig(Inet): min=120.2615 max=47790.6328 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 1 41 178 386 749 843 1526 2452 3378 3684 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.9 41.4 66.6 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3684 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3684 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5134954- 1127477 368 1877961.23 121.87 100.00 1125426- 622746 368 849239.56 102.96 100.00 622232- 265121 368 414560.87 94.39 100.00 264554- 169510 368 203042.96 71.80 100.00 169492- 119830 368 144289.86 51.20 100.00 119701- 91847 368 104656.10 35.64 100.00 91821- 65478 368 79642.49 28.95 100.00 65224- 5437 368 36714.95 18.98 100.00 5419- 2931 368 3872.02 5.27 97.28 2924- 750 372 2115.90 3.71 54.84 ------------------------------------------------------------------------------------ 5134954- 750 3684 371208.41 53.42 95.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 768924.95 93.67 100.00 1.41- 1.12 368 608244.70 63.42 99.46 1.12- 0.96 368 507016.20 71.26 97.55 0.96- 0.88 368 347130.39 59.61 94.57 0.88- 0.81 368 450552.07 68.90 99.46 0.81- 0.73 368 245657.64 41.23 95.65 0.73- 0.71 368 174690.29 34.23 88.59 0.71- 0.65 368 311472.73 47.45 94.02 0.65- 0.62 368 151187.14 27.18 87.50 0.62- 0.58 372 149616.55 27.56 94.89 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 371208.41 53.42 95.17 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:05:19 2018 Sorting 3684 observations 120 unique observations with > 7.00 F2/sig(F2) 3684 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 Total number of frames 628 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3684 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 Total number of frames 107 2957 observations > 7.00 F2/sig(F2) 2957 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 Total number of frames 107 Removing 'redundancy=1' reflections Average redundancy: 22.7 (Out of 2957 removed 3 = 2954, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 2954 observations in 6 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 Total number of frames 107 130 unique data precomputed (should be 130) 130 unique data with 2954 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 22.7 (Out of 2954 removed 0 = 2954, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 2954 observations RMS deviation of equivalent data = 0.24895 Rint = 0.17974 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17312, wR= 0.25399 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13042, wR= 0.16916, Acormin=0.618, Acormax=1.400, Acor_av=0.998 F test: Probability=1.000, F= 1.759 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11810, wR= 0.14824, Acormin=0.553, Acormax=1.441, Acor_av=0.912 F test: Probability=1.000, F= 1.218 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10557, wR= 0.14116, Acormin=0.654, Acormax=1.623, Acor_av=0.985 F test: Probability=1.000, F= 1.249 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09210, wR= 0.12166, Acormin=0.536, Acormax=1.562, Acor_av=0.899 F test: Probability=1.000, F= 1.312 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08035, wR= 0.10965, Acormin=0.509, Acormax=1.627, Acor_av=0.912 F test: Probability=1.000, F= 1.311 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09714, wR= 0.13311, Acormin=0.651, Acormax=1.703, Acor_av=0.990 F test: Probability=0.000, F= 0.683 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08513, wR= 0.11475, Acormin=0.519, Acormax=1.641, Acor_av=0.908 F test: Probability=0.000, F= 0.889 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07582, wR= 0.10525, Acormin=0.501, Acormax=1.663, Acor_av=0.918 F test: Probability=0.998, F= 1.118 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07250, wR= 0.09963, Acormin=0.390, Acormax=1.549, Acor_av=0.873 F test: Probability=0.988, F= 1.089 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09924, wR= 0.12925, Acormin=0.499, Acormax=1.501, Acor_av=0.855 F test: Probability=0.000, F= 0.534 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08400, wR= 0.11070, Acormin=0.510, Acormax=1.638, Acor_av=0.897 F test: Probability=0.000, F= 0.745 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08190, wR= 0.10766, Acormin=0.121, Acormax=0.436, Acor_av=0.237 F test: Probability=0.000, F= 0.782 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07441, wR= 0.09983, Acormin=0.120, Acormax=0.457, Acor_av=0.260 F test: Probability=0.000, F= 0.944 Trying model 14 (ne=8, no=7)... Results: Rint= 0.06974, wR= 0.09434, Acormin=0.130, Acormax=0.473, Acor_av=0.269 F test: Probability=0.958, F= 1.068 Final absorption model (ne=6, no=5): Rint= 0.07250, Acormin=0.390, Acormax=1.549, Acor_av=0.873 Combined refinement in use Rint: 0.17985 There are 107 active scales (one needs to be fixed) Refinement control: frame scale #71 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 154 pars with 11935 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24895 Using Levenberg-Marquardt: 0.00010 New wR= 0.06288 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17974 with corrections 0.05012 Rint for all data: 0.17985 with corrections 0.05035 0 observations identified as outliers and rejected Cycle 2 wR= 0.06288 Using Levenberg-Marquardt: 0.00001 New wR= 0.06004 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17974 with corrections 0.04747 Rint for all data: 0.17985 with corrections 0.04769 0 observations identified as outliers and rejected Cycle 3 wR= 0.06004 Using Levenberg-Marquardt: 0.00000 New wR= 0.05942 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17974 with corrections 0.04694 Rint for all data: 0.17985 with corrections 0.04717 0 observations identified as outliers and rejected Cycle 4 wR= 0.05942 Using Levenberg-Marquardt: 0.00000 New wR= 0.05912 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17974 with corrections 0.04668 Rint for all data: 0.17985 with corrections 0.04691 0 observations identified as outliers and rejected Cycle 5 wR= 0.05912 Using Levenberg-Marquardt: 0.00000 New wR= 0.05893 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17974 with corrections 0.04653 Rint for all data: 0.17985 with corrections 0.04676 0 observations identified as outliers and rejected Final wR= 0.05893 Final frame scales: Min= 0.7509 Max= 1.3062 Final absorption correction factors: Amin= 0.4938 Amax= 1.4223 PROFFIT INFO: Inet (after scale3 abspack): min=737.3601 max=4599395.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=143.9422 max=53205.1719 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/6 frame:1/109 3684 reflections read from tmp file 803 reflections are rejected (803 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 3 4 4 3 6 5 124 Initial Chi^2= 0.42932 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.94455 Current error model SIG(F2)^2 = 155.63*I_RAW + 0.00*I_BACK+(0.01587*)^2 Cycle 2, Chi^2= 1.01276 Current error model SIG(F2)^2 = 107.23*I_RAW + 0.00*I_BACK+(0.02234*)^2 Cycle 3, Chi^2= 1.00053 Current error model SIG(F2)^2 = 116.56*I_RAW + 0.00*I_BACK+(0.02064*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 115.65*I_RAW + 0.00*I_BACK+(0.02086*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 115.79*I_RAW + 0.00*I_BACK+(0.02082*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 115.79*I_RAW + 0.00*I_BACK+(0.02082*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4599396- 1098427 368 1778990.43 44.77 100.00 1096006- 604028 368 811690.23 37.63 100.00 603119- 256537 368 403479.91 36.07 100.00 256250- 153809 368 192551.38 31.77 100.00 153703- 124181 368 139090.21 25.61 100.00 124046- 87117 368 101327.83 19.63 100.00 87094- 67993 368 77760.70 16.83 100.00 67931- 4869 368 38768.42 12.00 100.00 4863- 2740 368 3593.04 4.63 96.47 2738- 737 372 2127.79 3.77 74.73 ------------------------------------------------------------------------------------ 4599396- 737 3684 354554.92 23.25 97.10 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 771675.64 36.68 100.00 1.41- 1.12 368 586679.84 28.72 99.46 1.12- 0.96 368 468493.64 27.83 98.64 0.96- 0.88 368 327039.29 23.82 97.28 0.88- 0.81 368 426864.60 27.37 99.73 0.81- 0.73 368 225521.14 18.90 96.74 0.73- 0.71 368 166878.05 17.45 91.85 0.71- 0.65 368 293635.04 22.33 97.83 0.65- 0.62 368 141997.35 14.51 92.39 0.62- 0.58 372 139106.47 14.98 97.04 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 354554.92 23.25 97.10 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 771675.64 36.68 100.00 4.82- 1.12 736 679177.74 32.70 99.73 4.82- 0.96 1104 608949.71 31.08 99.37 4.82- 0.88 1472 538472.10 29.26 98.85 4.82- 0.81 1840 516150.60 28.88 99.02 4.82- 0.73 2208 467712.36 27.22 98.64 4.82- 0.71 2576 424736.03 25.83 97.67 4.82- 0.65 2944 408348.40 25.39 97.69 4.82- 0.62 3312 378753.84 24.18 97.10 4.82- 0.58 3684 354554.92 23.25 97.10 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 354554.92 23.25 97.10 Scale applied to data: s=0.217420 (maximum obs:4599395.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.028: data 3684 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.028: data 3672 -> merged 157 Rejected total: 12, method kkm 9, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585891, 4.831385 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 21.50 100.00 301 1.41 - 1.12 14 14 30.29 100.00 424 1.12 - 0.97 14 14 30.14 100.00 422 0.96 - 0.84 14 14 32.29 100.00 452 0.84 - 0.78 14 14 24.57 100.00 344 0.78 - 0.73 14 14 25.93 100.00 363 0.73 - 0.69 14 14 24.00 100.00 336 0.69 - 0.66 14 14 20.79 100.00 291 0.65 - 0.63 14 14 21.43 100.00 300 0.63 - 0.60 14 14 19.07 100.00 267 --------------------------------------------------------------- 8.37 - 0.60 140 140 25.00 100.00 3500 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:05:20 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361315 8.374596 8.368708 90.0147 90.0321 89.9969 3672 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1876 0 2463 2463 3672 N (int>3sigma) = 0 0 0 0 1876 0 2391 2385 3565 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.4 79.5 77.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.00 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.913 5.917 5.917 119.96 119.96 90.05 Niggli form: a.a = 34.967 b.b = 35.006 c.c = 35.009 b.c = -17.482 a.c = -17.472 a.b = -0.031 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.054 CUBIC F-lattice R(int) = 0.047 [ 3515] Vol = 586.0 Cell: 8.375 8.369 8.361 89.97 90.00 90.01 Volume: 586.00 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.060 TETRAGONAL I-lattice R(int) = 0.045 [ 3265] Vol = 293.0 Cell: 5.920 5.919 8.361 90.02 89.98 89.96 Volume: 293.00 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.051 TETRAGONAL I-lattice R(int) = 0.045 [ 3259] Vol = 293.0 Cell: 5.913 5.917 8.375 89.99 90.01 90.05 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.021 TETRAGONAL I-lattice R(int) = 0.045 [ 3265] Vol = 293.0 Cell: 5.919 5.920 8.361 90.02 90.02 90.04 Volume: 293.00 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.041 ORTHORHOMBIC F-lattice R(int) = 0.044 [ 3223] Vol = 586.0 Cell: 8.361 8.369 8.375 90.01 90.00 89.97 Volume: 586.00 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 3210] Vol = 293.0 Cell: 8.361 5.919 5.920 89.96 89.98 90.02 Volume: 293.00 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.039 ORTHORHOMBIC I-lattice R(int) = 0.044 [ 3209] Vol = 293.0 Cell: 5.913 5.917 8.375 90.01 89.99 90.05 Volume: 293.00 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.041 MONOCLINIC I-lattice R(int) = 0.043 [ 2876] Vol = 293.0 Cell: 5.919 8.361 5.920 90.02 90.04 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.040 MONOCLINIC I-lattice R(int) = 0.043 [ 2874] Vol = 293.0 Cell: 5.917 8.369 5.917 89.97 90.09 89.99 Volume: 293.00 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.043 [ 2876] Vol = 293.0 Cell: 5.919 8.361 5.920 90.02 90.04 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 2861] Vol = 293.0 Cell: 5.917 5.913 8.375 90.01 90.01 89.95 Volume: 293.00 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.006 MONOCLINIC I-lattice R(int) = 0.043 [ 2873] Vol = 293.0 Cell: 5.913 8.375 5.917 89.99 90.05 90.01 Volume: 293.00 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.009 MONOCLINIC I-lattice R(int) = 0.043 [ 2873] Vol = 293.0 Cell: 5.913 8.375 5.917 90.01 90.05 89.99 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2186] Vol = 146.5 Cell: 5.913 5.917 5.917 119.96 119.96 90.05 Volume: 146.50 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1876 0 2459 2463 3672 N (int>3sigma) = 0 0 0 0 1876 0 2386 2385 3565 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 76.7 79.5 77.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.3 23.5 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.176 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 275 821 N I>3s 37 37 262 821 0.9 0.9 0.7 36.2 9.0 9.0 5.4 26.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.046 3260 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3299 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.374596 8.368708 8.361315 89.9679 90.0031 90.0147 ZERR 3.00 0.000630 0.000487 0.000593 0.0053 0.0059 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3990306- 745832 602 600 26 23.1 1433855.96 42.46 0.041 0.055 735324- 224147 573 572 26 22.0 447507.14 36.19 0.061 0.080 219670- 96556 850 850 26 32.7 147726.06 26.32 0.043 0.056 94353- 69647 589 588 26 22.6 81824.66 17.07 0.069 0.089 65440- 3570 477 473 26 18.2 26176.73 9.17 0.083 0.105 3388- 1718 593 589 27 21.8 2643.99 4.25 0.198 0.256 ------------------------------------------------------------------------------------------- 3990306- 1718 3684 3672 157 23.4 355094.39 23.26 0.047 0.062 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 689 684 26 26.3 622717.93 31.99 0.047 0.063 0.023 1.12-0.88 813 811 26 31.2 457980.54 27.04 0.034 0.046 0.026 0.85-0.75 684 684 26 26.3 325951.29 22.68 0.042 0.053 0.029 0.74-0.68 598 596 26 22.9 255208.45 20.33 0.058 0.068 0.033 0.67-0.63 566 566 26 21.8 146478.64 16.00 0.075 0.092 0.042 0.62-0.59 334 331 27 12.3 146777.95 14.88 0.074 0.086 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3684 3672 157 23.4 355094.39 23.26 0.047 0.062 0.028 inf-0.60 3508 3498 139 25.2 367300.64 23.73 0.046 0.061 0.027 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 684 26 26 100.0 26.3 622717.93 177.97 0.047 0.005 1.12-0.88 811 26 26 100.0 31.2 457980.54 153.86 0.034 0.005 0.85-0.75 684 26 26 100.0 26.3 325951.29 123.20 0.042 0.006 0.74-0.68 596 26 26 100.0 22.9 255208.45 99.69 0.058 0.008 0.67-0.63 566 26 26 100.0 21.8 146478.64 74.01 0.075 0.009 0.62-0.59 331 27 27 100.0 12.3 146777.95 60.16 0.074 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3672 157 157 100.0 23.4 355094.39 123.09 0.047 0.007 inf-0.60 3498 139 139 100.0 25.2 367300.64 126.73 0.046 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025035 -0.079418 -0.015578 ( 0.000006 0.000006 0.000006 ) 0.072509 -0.029213 0.032909 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003579 0.076537 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000000 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000002 0.007184 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025035 -0.079418 -0.015578 ( 0.000006 0.000006 0.000006 ) 0.072509 -0.029213 0.032909 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003579 0.076537 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3613(6) 8.3747(6) 8.3687(5) 90.015(5) 90.032(5) 89.997(6) V = 586.01(7) unit cell: 8.36823(18) 8.36823(18) 8.36823(18) 90.0 90.0 90.0 V = 586.01(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.918) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.757) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.757) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.757) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) PROFFIT INFO: signal sum: min=255.0000 max=23168420.0000 PROFFIT INFO: signal sum lp corr: min=468.6985 max=3209345.9464 PROFFIT INFO: background sum: min=612.0000 max=26130.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=51 max=501 PROFFIT INFO: Inet: min=749.9176 max=5134953.5000 PROFFIT INFO: sig(Inet): min=120.2615 max=47790.6328 PROFFIT INFO: Inet/sig(Inet): min=0.96 max=248.69 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 82 356 772 1498 1686 3052 4904 6756 7368 Percent 0.0 0.0 1.1 4.8 10.5 20.3 22.9 41.4 66.6 91.7 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3684 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3684 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5134954- 1127477 368 1877961.23 121.87 100.00 1125426- 622746 368 849239.56 102.96 100.00 622232- 265121 368 414560.87 94.39 100.00 264554- 169510 368 203042.96 71.80 100.00 169492- 119830 368 144289.86 51.20 100.00 119701- 91847 368 104656.10 35.64 100.00 91821- 65478 368 79642.49 28.95 100.00 65224- 5437 368 36714.95 18.98 100.00 5419- 2931 368 3872.02 5.27 97.28 2924- 750 372 2115.90 3.71 54.84 ------------------------------------------------------------------------------------ 5134954- 750 3684 371208.41 53.42 95.17 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 768924.95 93.67 100.00 1.41- 1.12 368 608244.70 63.42 99.46 1.12- 0.96 368 507016.20 71.26 97.55 0.96- 0.88 368 347130.39 59.61 94.57 0.88- 0.81 368 450552.07 68.90 99.46 0.81- 0.73 368 245657.64 41.23 95.65 0.73- 0.71 368 174690.29 34.23 88.59 0.71- 0.65 368 311472.73 47.45 94.02 0.65- 0.62 368 151187.14 27.18 87.50 0.62- 0.58 372 149616.55 27.56 94.89 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 371208.41 53.42 95.17 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:05:21 2018 Sorting 3684 observations 86 unique observations with > 7.00 F2/sig(F2) 3684 observations in 6 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 Total number of frames 628 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3684 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 Total number of frames 82 2957 observations > 7.00 F2/sig(F2) 2957 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 Total number of frames 82 Removing 'redundancy=1' reflections Average redundancy: 31.8 (Out of 2957 removed 3 = 2954, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 2954 observations in 6 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 Total number of frames 82 93 unique data precomputed (should be 93) 93 unique data with 2954 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 31.8 (Out of 2954 removed 0 = 2954, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 2954 observations RMS deviation of equivalent data = 0.24933 Rint = 0.17998 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.17330, wR= 0.25435 Trying model 1 (ne=2, no=0)... Results: Rint= 0.13041, wR= 0.16965, Acormin=0.617, Acormax=1.400, Acor_av=0.998 F test: Probability=1.000, F= 1.763 Trying model 2 (ne=2, no=1)... Results: Rint= 0.11847, wR= 0.14881, Acormin=0.553, Acormax=1.441, Acor_av=0.912 F test: Probability=1.000, F= 1.210 Trying model 3 (ne=4, no=0)... Results: Rint= 0.10582, wR= 0.14166, Acormin=0.655, Acormax=1.624, Acor_av=0.985 F test: Probability=1.000, F= 1.251 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09236, wR= 0.12222, Acormin=0.535, Acormax=1.561, Acor_av=0.898 F test: Probability=1.000, F= 1.311 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08038, wR= 0.11019, Acormin=0.508, Acormax=1.626, Acor_av=0.911 F test: Probability=1.000, F= 1.317 Trying model 6 (ne=6, no=0)... Results: Rint= 0.09695, wR= 0.13336, Acormin=0.651, Acormax=1.708, Acor_av=0.992 F test: Probability=0.000, F= 0.687 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08520, wR= 0.11501, Acormin=0.520, Acormax=1.643, Acor_av=0.909 F test: Probability=0.000, F= 0.888 Trying model 8 (ne=6, no=3)... Results: Rint= 0.07585, wR= 0.10552, Acormin=0.502, Acormax=1.666, Acor_av=0.918 F test: Probability=0.998, F= 1.118 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07269, wR= 0.09998, Acormin=0.394, Acormax=1.552, Acor_av=0.874 F test: Probability=0.984, F= 1.085 Trying model 10 (ne=8, no=0)... Results: Rint= 0.09929, wR= 0.12967, Acormin=0.507, Acormax=1.508, Acor_av=0.857 F test: Probability=0.000, F= 0.537 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08396, wR= 0.11094, Acormin=0.512, Acormax=1.643, Acor_av=0.898 F test: Probability=0.000, F= 0.750 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08204, wR= 0.10820, Acormin=0.120, Acormax=0.433, Acor_av=0.235 F test: Probability=0.000, F= 0.783 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07456, wR= 0.10048, Acormin=0.120, Acormax=0.452, Acor_av=0.257 F test: Probability=0.000, F= 0.945 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07000, wR= 0.09489, Acormin=0.128, Acormax=0.468, Acor_av=0.266 F test: Probability=0.954, F= 1.066 Final absorption model (ne=6, no=5): Rint= 0.07269, Acormin=0.394, Acormax=1.552, Acor_av=0.874 Combined refinement in use Rint: 0.18008 There are 82 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 129 pars with 8385 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.24933 Using Levenberg-Marquardt: 0.00010 New wR= 0.06456 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17998 with corrections 0.05097 Rint for all data: 0.18008 with corrections 0.05119 0 observations identified as outliers and rejected Cycle 2 wR= 0.06456 Using Levenberg-Marquardt: 0.00001 New wR= 0.06153 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17998 with corrections 0.04854 Rint for all data: 0.18008 with corrections 0.04877 0 observations identified as outliers and rejected Cycle 3 wR= 0.06153 Using Levenberg-Marquardt: 0.00000 New wR= 0.06070 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17998 with corrections 0.04793 Rint for all data: 0.18008 with corrections 0.04815 0 observations identified as outliers and rejected Cycle 4 wR= 0.06070 Using Levenberg-Marquardt: 0.00000 New wR= 0.06026 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17998 with corrections 0.04761 Rint for all data: 0.18008 with corrections 0.04783 0 observations identified as outliers and rejected Cycle 5 wR= 0.06026 Using Levenberg-Marquardt: 0.00000 New wR= 0.05998 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.17998 with corrections 0.04742 Rint for all data: 0.18008 with corrections 0.04765 0 observations identified as outliers and rejected Final wR= 0.05998 Final frame scales: Min= 0.7923 Max= 1.2765 Final absorption correction factors: Amin= 0.4845 Amax= 1.3828 PROFFIT INFO: Inet (after scale3 abspack): min=752.3530 max=4633565.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=144.2083 max=53082.8281 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/6 frame:1/109 3684 reflections read from tmp file 800 reflections are rejected (800 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 2 3 3 2 1 4 4 88 Initial Chi^2= 0.41375 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 1.38211 Current error model SIG(F2)^2 = 169.94*I_RAW + 0.00*I_BACK+(0.00846*)^2 Cycle 2, Chi^2= 1.21274 Current error model SIG(F2)^2 = 68.57*I_RAW + 0.00*I_BACK+(0.02701*)^2 Cycle 3, Chi^2= 1.00072 Current error model SIG(F2)^2 = 113.94*I_RAW + 0.00*I_BACK+(0.02178*)^2 Cycle 4, Chi^2= 0.99997 Current error model SIG(F2)^2 = 112.62*I_RAW + 0.00*I_BACK+(0.02207*)^2 Cycle 5, Chi^2= 1.00001 Current error model SIG(F2)^2 = 112.88*I_RAW + 0.00*I_BACK+(0.02201*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 112.88*I_RAW + 0.00*I_BACK+(0.02201*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4633566- 1098512 368 1779382.12 42.74 100.00 1095174- 603500 368 812002.04 36.55 100.00 601792- 257132 368 403258.64 35.03 100.00 257129- 153764 368 192547.93 31.11 100.00 153703- 123984 368 139184.59 25.36 100.00 123981- 87022 368 101256.11 19.63 100.00 87009- 67617 368 77784.91 16.91 100.00 67490- 4894 368 38830.04 12.04 100.00 4878- 2738 368 3592.56 4.70 97.28 2730- 752 372 2129.11 3.83 76.34 ------------------------------------------------------------------------------------ 4633566- 752 3684 354613.67 22.77 97.34 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 770672.12 35.30 100.00 1.41- 1.12 368 587444.29 27.84 99.46 1.12- 0.96 368 468556.17 27.12 98.64 0.96- 0.88 368 327638.08 23.35 97.55 0.88- 0.81 368 426769.15 26.79 99.73 0.81- 0.73 368 225921.97 18.64 97.01 0.73- 0.71 368 167076.18 17.33 92.66 0.71- 0.65 368 293251.68 22.04 97.83 0.65- 0.62 368 141974.29 14.44 92.93 0.62- 0.58 372 139174.49 14.93 97.58 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 354613.67 22.77 97.34 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 368 770672.12 35.30 100.00 4.82- 1.12 736 679058.21 31.57 99.73 4.82- 0.96 1104 608890.86 30.08 99.37 4.82- 0.88 1472 538577.66 28.40 98.91 4.82- 0.81 1840 516215.96 28.08 99.08 4.82- 0.73 2208 467833.63 26.50 98.73 4.82- 0.71 2576 424868.28 25.19 97.86 4.82- 0.65 2944 408416.20 24.80 97.86 4.82- 0.62 3312 378811.55 23.65 97.31 4.82- 0.58 3684 354613.67 22.77 97.34 ------------------------------------------------------------------------------------ 4.82- 0.58 3684 354613.67 22.77 97.34 Scale applied to data: s=0.215816 (maximum obs:4633565.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.029: data 3684 -> merged 110 With outlier rejection... Rint 0.047; Rsigma 0.029: data 3671 -> merged 110 Rejected total: 13, method kkm 10, method Blessing 3 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585894, 4.831402 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 22.90 100.00 229 1.61 - 1.21 10 10 33.80 100.00 338 1.17 - 1.01 10 10 43.80 100.00 438 0.99 - 0.89 10 10 42.40 100.00 424 0.88 - 0.81 10 10 40.80 100.00 408 0.81 - 0.74 10 10 35.60 100.00 356 0.73 - 0.71 10 10 38.70 100.00 387 0.70 - 0.66 10 10 32.80 100.00 328 0.66 - 0.64 10 10 30.00 100.00 300 0.63 - 0.60 10 10 29.00 100.00 290 --------------------------------------------------------------- 8.37 - 0.60 100 100 34.98 100.00 3498 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:05:20 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361315 8.374596 8.368708 90.0147 90.0321 89.9969 3672 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1876 0 2463 2463 3672 N (int>3sigma) = 0 0 0 0 1876 0 2391 2385 3565 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 77.4 79.5 77.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.4 23.5 23.3 Lattice type: F chosen Volume: 586.00 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.913 5.917 5.917 119.96 119.96 90.05 Niggli form: a.a = 34.967 b.b = 35.006 c.c = 35.009 b.c = -17.482 a.c = -17.472 a.b = -0.031 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.054 CUBIC F-lattice R(int) = 0.047 [ 3515] Vol = 586.0 Cell: 8.375 8.369 8.361 89.97 90.00 90.01 Volume: 586.00 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.060 TETRAGONAL I-lattice R(int) = 0.045 [ 3265] Vol = 293.0 Cell: 5.920 5.919 8.361 90.02 89.98 89.96 Volume: 293.00 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.051 TETRAGONAL I-lattice R(int) = 0.045 [ 3259] Vol = 293.0 Cell: 5.913 5.917 8.375 89.99 90.01 90.05 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.021 TETRAGONAL I-lattice R(int) = 0.045 [ 3265] Vol = 293.0 Cell: 5.919 5.920 8.361 90.02 90.02 90.04 Volume: 293.00 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.041 ORTHORHOMBIC F-lattice R(int) = 0.044 [ 3223] Vol = 586.0 Cell: 8.361 8.369 8.375 90.01 90.00 89.97 Volume: 586.00 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.063 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 3210] Vol = 293.0 Cell: 8.361 5.919 5.920 89.96 89.98 90.02 Volume: 293.00 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.039 ORTHORHOMBIC I-lattice R(int) = 0.044 [ 3209] Vol = 293.0 Cell: 5.913 5.917 8.375 90.01 89.99 90.05 Volume: 293.00 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.041 MONOCLINIC I-lattice R(int) = 0.043 [ 2876] Vol = 293.0 Cell: 5.919 8.361 5.920 90.02 90.04 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.040 MONOCLINIC I-lattice R(int) = 0.043 [ 2874] Vol = 293.0 Cell: 5.917 8.369 5.917 89.97 90.09 89.99 Volume: 293.00 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.041 MONOCLINIC I-lattice R(int) = 0.043 [ 2876] Vol = 293.0 Cell: 5.919 8.361 5.920 90.02 90.04 90.02 Volume: 293.00 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 2861] Vol = 293.0 Cell: 5.917 5.913 8.375 90.01 90.01 89.95 Volume: 293.00 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.006 MONOCLINIC I-lattice R(int) = 0.043 [ 2873] Vol = 293.0 Cell: 5.913 8.375 5.917 89.99 90.05 90.01 Volume: 293.00 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.009 MONOCLINIC I-lattice R(int) = 0.043 [ 2873] Vol = 293.0 Cell: 5.913 8.375 5.917 90.01 90.05 89.99 Volume: 293.00 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2186] Vol = 146.5 Cell: 5.913 5.917 5.917 119.96 119.96 90.05 Volume: 146.50 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1876 0 2459 2463 3672 N (int>3sigma) = 0 0 0 0 1876 0 2386 2385 3565 Mean intensity = 0.0 0.0 0.0 0.0 30.5 0.0 76.7 79.5 77.2 Mean int/sigma = 0.0 0.0 0.0 0.0 24.0 0.0 23.3 23.5 23.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.176 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 37 37 275 821 N I>3s 37 37 262 821 0.9 0.9 0.7 36.2 9.0 9.0 5.4 26.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.046 3260 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3299 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.374596 8.368708 8.361315 89.9679 90.0031 90.0147 ZERR 3.00 0.000630 0.000487 0.000593 0.0053 0.0059 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3998227- 509757 816 814 27 30.1 1224569.83 38.88 0.045 0.062 506390- 119416 1095 1094 27 40.5 213788.33 29.94 0.050 0.066 105279- 35512 907 905 27 33.5 77996.43 16.88 0.068 0.087 10323- 1831 866 858 29 29.6 3446.71 4.62 0.168 0.210 ------------------------------------------------------------------------------------------- 3998227- 1831 3684 3671 110 33.4 355278.76 22.78 0.047 0.064 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 934 929 27 34.4 641193.91 31.72 0.045 0.064 0.024 1.01-0.78 1130 1127 28 40.3 325747.53 22.03 0.038 0.047 0.029 0.76-0.65 974 972 28 34.7 244871.80 19.41 0.056 0.067 0.034 0.65-0.59 646 643 27 23.8 160849.65 16.30 0.078 0.096 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3684 3671 110 33.4 355278.76 22.78 0.047 0.064 0.029 inf-0.60 3508 3496 99 35.3 367483.66 23.23 0.047 0.062 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 929 27 27 100.0 34.4 641193.91 208.89 0.045 0.006 1.01-0.78 1127 28 28 100.0 40.3 325747.53 149.83 0.038 0.005 0.76-0.65 972 28 28 100.0 34.7 244871.80 122.13 0.056 0.007 0.65-0.59 643 27 27 100.0 23.8 160849.65 91.72 0.078 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3671 110 110 100.0 33.4 355278.76 147.26 0.047 0.006 inf-0.60 3496 99 99 100.0 35.3 367483.66 151.11 0.047 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:11:20 2018) ID: 2932; threads 39; handles 876; mem 517968.00 (1237704.00)kB; time: 1w 5d 1h 16m 51s MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:505.8,peak PF: 697.1, WS: 296.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:228.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:507.6,peak PF: 697.1, WS: 298.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:11:20 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00059 ) 8.37691 ( 0.00063 ) 8.37554 ( 0.00049 ) 90.02113 ( 0.00543 ) 90.03240 ( 0.00527 ) 90.03043 ( 0.00590 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:11:20 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000000 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 0.007173 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000002 0.007184 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(5) 90.021(5) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.36823(18) 8.36823(18) 8.36823(18) 90.0 90.0 90.0 V = 586.01(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 488 peaks identified as outliers and rejected 481 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 481 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 481 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.020 ( 0.237) | 1.201 ( 0.650) | 1.103 ( 0.625) | 1.41- 1.17 | 48 | 1.034 ( 0.130) | 1.135 ( 0.446) | 0.960 ( 0.494) | 1.17- 1.01 | 48 | 0.999 ( 0.093) | 1.041 ( 0.221) | 1.001 ( 0.449) | 1.01- 0.92 | 48 | 1.023 ( 0.070) | 1.023 ( 0.106) | 1.097 ( 0.438) | 0.92- 0.82 | 48 | 1.001 ( 0.082) | 0.980 ( 0.110) | 1.110 ( 0.379) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.963 ( 0.114) | 1.085 ( 0.438) | 0.75- 0.71 | 48 | 0.985 ( 0.046) | 0.917 ( 0.069) | 1.218 ( 0.499) | 0.71- 0.67 | 48 | 0.952 ( 0.047) | 0.863 ( 0.057) | 1.215 ( 0.481) | 0.66- 0.62 | 48 | 0.935 ( 0.047) | 0.847 ( 0.039) | 1.198 ( 0.425) | 0.62- 0.59 | 49 | 0.903 ( 0.042) | 0.812 ( 0.038) | 1.369 ( 0.581) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 481 | 0.985 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb PROFFITPEAK info: 243 peaks in the peak location table UB fit with 117 obs out of 124 (total:124,skipped:0) (94.35%) UB - matrix: -0.024910 -0.079718 -0.015726 ( 0.000101 0.000099 0.000080 ) 0.072365 -0.029626 0.032895 ( 0.000123 0.000120 0.000097 ) -0.036537 -0.003171 0.076759 ( 0.000127 0.000124 0.000100 ) M - matrix: 0.007192 -0.000042 -0.000032 ( 0.000021 0.000013 0.000013 ) -0.000042 0.007243 0.000036 ( 0.000013 0.000017 0.000013 ) -0.000032 0.000036 0.007221 ( 0.000013 0.000013 0.000017 ) unit cell: 8.364(11) 8.335(10) 8.347(11) 90.28(10) 89.74(11) 89.67(10) V = 582(1) UB fit with 117 obs out of 124 (total:124,skipped:0) (94.35%) UB - matrix: -0.024910 -0.079718 -0.015726 ( 0.000101 0.000099 0.000080 ) 0.072365 -0.029626 0.032895 ( 0.000123 0.000120 0.000097 ) -0.036537 -0.003171 0.076759 ( 0.000127 0.000124 0.000100 ) M - matrix: 0.007192 -0.000042 -0.000032 ( 0.000021 0.000013 0.000013 ) -0.000042 0.007243 0.000036 ( 0.000013 0.000017 0.000013 ) -0.000032 0.000036 0.007221 ( 0.000013 0.000013 0.000017 ) unit cell: 8.364(11) 8.335(10) 8.347(11) 90.28(10) 89.74(11) 89.67(10) V = 582(1) OTKP changes: 25 1 1 1 No constraint UB - matrix: -0.025082 -0.079397 -0.015594 ( 0.000102 0.000100 0.000081 ) 0.072279 -0.029827 0.032640 ( 0.000116 0.000114 0.000092 ) -0.036399 -0.003136 0.076552 ( 0.000125 0.000122 0.000099 ) M - matrix: 0.007178 -0.000050 -0.000036 ( 0.000020 0.000013 0.000013 ) -0.000050 0.007203 0.000025 ( 0.000013 0.000017 0.000012 ) -0.000036 0.000025 0.007169 ( 0.000013 0.000012 0.000016 ) Constraint UB - matrix: -0.025082 -0.079397 -0.015594 ( 0.000102 0.000100 0.000081 ) 0.072279 -0.029827 0.032640 ( 0.000116 0.000114 0.000092 ) -0.036399 -0.003136 0.076552 ( 0.000125 0.000122 0.000099 ) M - matrix: 0.007137 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007137 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007137 ( 0.000000 0.000000 0.000002 ) UB fit with 117 obs out of 124 (total:124,skipped:0) (94.35%) unit cell: 8.372(11) 8.357(10) 8.377(10) 90.19(10) 89.71(10) 89.60(10) V = 586(1) unit cell: 8.3689(11) 8.3689(11) 8.3689(11) 90.0 90.0 90.0 V = 586.15(13) UB fit with 117 obs out of 124 (total:124,skipped:0) (94.35%) UB - matrix: -0.025082 -0.079397 -0.015594 ( 0.000102 0.000100 0.000081 ) 0.072279 -0.029827 0.032640 ( 0.000116 0.000114 0.000092 ) -0.036399 -0.003136 0.076552 ( 0.000125 0.000122 0.000099 ) M - matrix: 0.007178 -0.000050 -0.000036 ( 0.000020 0.000013 0.000013 ) -0.000050 0.007203 0.000025 ( 0.000013 0.000017 0.000012 ) -0.000036 0.000025 0.007169 ( 0.000013 0.000012 0.000016 ) unit cell: 8.372(11) 8.357(10) 8.377(10) 90.19(10) 89.71(10) 89.60(10) V = 586(1) OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 OTKP changes: 24 1 1 1 124 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Run 7 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=53.064) HKL list info: 264 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025082 -0.079397 -0.015594 ( 0.000102 0.000100 0.000081 ) 0.072279 -0.029827 0.032640 ( 0.000116 0.000114 0.000092 ) -0.036399 -0.003136 0.076552 ( 0.000125 0.000122 0.000099 ) M - matrix: 0.007178 -0.000050 -0.000036 ( 0.000020 0.000013 0.000013 ) -0.000050 0.007203 0.000025 ( 0.000013 0.000017 0.000012 ) -0.000036 0.000025 0.007169 ( 0.000013 0.000012 0.000016 ) Constraint UB - matrix: -0.025082 -0.079397 -0.015594 ( 0.000102 0.000100 0.000081 ) 0.072279 -0.029827 0.032640 ( 0.000116 0.000114 0.000092 ) -0.036399 -0.003136 0.076552 ( 0.000125 0.000122 0.000099 ) M - matrix: 0.007137 0.000000 0.000000 ( 0.000002 0.000000 0.000000 ) 0.000000 0.007137 0.000000 ( 0.000000 0.000002 0.000000 ) 0.000000 0.000000 0.007137 ( 0.000000 0.000000 0.000002 ) UB fit with 117 obs out of 124 (total:124,skipped:0) (94.35%) unit cell: 8.372(11) 8.357(10) 8.377(10) 90.19(10) 89.71(10) 89.60(10) V = 586(1) unit cell: 8.3689(11) 8.3689(11) 8.3689(11) 90.0 90.0 90.0 V = 586.15(13) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 118 obs out of 124 (total:124,skipped:0) (95.16%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb 2 of 95 peaks identified as outliers and rejected 93 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 93 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 93 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.09- 1.60 | 9 | 1.049 ( 0.091) | 1.307 ( 0.478) | 1.168 ( 0.676) | 1.42- 1.26 | 9 | 1.017 ( 0.100) | 1.217 ( 0.550) | 0.893 ( 0.484) | 1.21- 0.99 | 9 | 0.996 ( 0.105) | 1.001 ( 0.119) | 1.028 ( 0.410) | 0.97- 0.89 | 9 | 1.021 ( 0.078) | 0.999 ( 0.101) | 0.913 ( 0.249) | 0.84- 0.82 | 9 | 1.018 ( 0.086) | 1.036 ( 0.116) | 1.209 ( 0.588) | 0.82- 0.74 | 9 | 0.983 ( 0.102) | 0.914 ( 0.111) | 1.107 ( 0.463) | 0.73- 0.71 | 9 | 0.962 ( 0.052) | 0.865 ( 0.055) | 1.475 ( 0.751) | 0.71- 0.67 | 9 | 0.979 ( 0.021) | 0.877 ( 0.044) | 1.332 ( 0.602) | 0.67- 0.64 | 9 | 0.978 ( 0.037) | 0.837 ( 0.058) | 1.199 ( 0.462) | 0.64- 0.59 | 12 | 0.915 ( 0.035) | 0.767 ( 0.037) | 1.229 ( 0.459) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.09- 0.59 | 93 | 0.989 ( 0.085) | 0.975 ( 0.290) | 1.158 ( 0.556) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) UB - matrix: -0.025156 -0.079301 -0.015645 ( 0.000067 0.000061 0.000053 ) 0.072248 -0.029570 0.032807 ( 0.000074 0.000068 0.000059 ) -0.036237 -0.003162 0.076527 ( 0.000080 0.000073 0.000063 ) M - matrix: 0.007166 -0.000027 -0.000009 ( 0.000013 0.000008 0.000008 ) -0.000027 0.007173 0.000029 ( 0.000008 0.000010 0.000008 ) -0.000009 0.000029 0.007178 ( 0.000008 0.000008 0.000011 ) unit cell: 8.379(7) 8.375(6) 8.372(7) 90.23(6) 89.93(7) 89.79(6) V = 587.5(8) OTKP changes: 93 1 1 1 No constraint UB - matrix: -0.025112 -0.079398 -0.015793 ( 0.000066 0.000061 0.000053 ) 0.072356 -0.029693 0.032663 ( 0.000067 0.000061 0.000053 ) -0.036234 -0.003450 0.076505 ( 0.000076 0.000069 0.000060 ) M - matrix: 0.007179 -0.000030 -0.000012 ( 0.000012 0.000008 0.000008 ) -0.000030 0.007198 0.000020 ( 0.000008 0.000010 0.000007 ) -0.000012 0.000020 0.007169 ( 0.000008 0.000007 0.000010 ) Constraint UB - matrix: -0.025112 -0.079398 -0.015793 ( 0.000066 0.000061 0.000053 ) 0.072356 -0.029693 0.032663 ( 0.000067 0.000061 0.000053 ) -0.036234 -0.003450 0.076505 ( 0.000076 0.000069 0.000060 ) M - matrix: 0.007161 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007161 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007161 ( 0.000000 0.000000 0.000001 ) UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) unit cell: 8.372(6) 8.361(6) 8.377(6) 90.16(6) 89.90(6) 89.76(6) V = 586.3(7) unit cell: 8.3697(7) 8.3697(7) 8.3697(7) 90.0 90.0 90.0 V = 586.32(8) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.980) HKL list info: 266 refl (0 shortened) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 93 obs out of 93 (total:93,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with average model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb 1 of 95 peaks identified as outliers and rejected 94 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 94 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 94 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.61 | 9 | 1.093 ( 0.201) | 1.327 ( 0.525) | 1.322 ( 0.731) | 1.41- 1.21 | 9 | 1.020 ( 0.082) | 1.179 ( 0.341) | 0.951 ( 0.473) | 1.12- 0.97 | 9 | 0.989 ( 0.099) | 0.985 ( 0.109) | 1.003 ( 0.343) | 0.97- 0.89 | 9 | 1.030 ( 0.082) | 1.006 ( 0.105) | 0.967 ( 0.375) | 0.84- 0.82 | 9 | 1.040 ( 0.058) | 1.056 ( 0.094) | 1.276 ( 0.586) | 0.82- 0.75 | 9 | 0.970 ( 0.113) | 0.913 ( 0.114) | 1.053 ( 0.444) | 0.74- 0.72 | 9 | 0.959 ( 0.052) | 0.865 ( 0.055) | 1.363 ( 0.653) | 0.71- 0.68 | 9 | 0.983 ( 0.022) | 0.894 ( 0.057) | 1.347 ( 0.642) | 0.67- 0.64 | 9 | 0.976 ( 0.037) | 0.838 ( 0.056) | 1.346 ( 0.550) | 0.64- 0.59 | 13 | 0.923 ( 0.041) | 0.773 ( 0.040) | 1.208 ( 0.448) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 94 | 0.995 ( 0.103) | 0.975 ( 0.263) | 1.185 ( 0.558) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 282 | 1.115 ( 0.126) | 1.237 ( 0.465) | 1.257 ( 1.073) | 12.9-18.6 | 282 | 1.075 ( 0.052) | 1.121 ( 0.221) | 1.170 ( 0.514) | 18.7-22.9 | 282 | 1.064 ( 0.074) | 1.138 ( 0.378) | 1.162 ( 0.541) | 22.9-27.1 | 282 | 1.032 ( 0.088) | 1.073 ( 0.280) | 1.147 ( 0.559) | 27.1-30.7 | 282 | 1.008 ( 0.073) | 1.012 ( 0.261) | 1.201 ( 0.491) | 30.7-33.8 | 282 | 0.973 ( 0.075) | 0.928 ( 0.107) | 1.184 ( 0.513) | 33.8-36.9 | 282 | 0.955 ( 0.071) | 0.901 ( 0.100) | 1.150 ( 0.470) | 36.9-39.7 | 282 | 0.936 ( 0.081) | 0.870 ( 0.134) | 1.217 ( 0.553) | 39.7-42.7 | 282 | 0.919 ( 0.073) | 0.837 ( 0.090) | 1.189 ( 0.538) | 42.7-50.0 | 279 | 0.922 ( 0.082) | 0.811 ( 0.066) | 1.166 ( 0.479) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.0 | 2817 | 1.000 ( 0.105) | 0.993 ( 0.282) | 1.184 ( 0.598) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0018 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:11:57 2018 PROFFITMAIN - Started at Tue Mar 27 16:11:57 2018 OTKP changes: 2809 2 4 6 OTKP changes: 2809 2 4 6 No constraint UB - matrix: -0.025048 -0.079518 -0.015606 ( 0.000005 0.000006 0.000006 ) 0.072512 -0.029244 0.032943 ( 0.000005 0.000006 0.000006 ) -0.036229 -0.003593 0.076559 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007198 0.000001 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000001 0.007191 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000002 0.007190 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025048 -0.079518 -0.015606 ( 0.000005 0.000006 0.000006 ) 0.072512 -0.029244 0.032943 ( 0.000005 0.000006 0.000006 ) -0.036229 -0.003593 0.076559 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) UB fit with 2812 obs out of 2817 (total:2817,skipped:0) (99.82%) unit cell: 8.3604(5) 8.3642(6) 8.3649(4) 90.019(5) 90.047(5) 90.011(5) V = 584.95(6) unit cell: 8.36319(14) 8.36319(14) 8.36319(14) 90.0 90.0 90.0 V = 584.946(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024871 -0.079572 -0.015659 ( 0.000013 0.000015 0.000011 ) 0.072445 -0.029200 0.032953 ( 0.000016 0.000018 0.000013 ) -0.036290 -0.003653 0.076364 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007184 -0.000004 0.000005 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007198 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000005 0.000005 0.007163 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3686(15) 8.3605(15) 8.3810(10) 90.039(12) 90.044(12) 89.970(14) V = 586.39(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 479 obs out of 481 (total:481,skipped:0) (99.58%) UB - matrix: -0.024979 -0.079532 -0.015506 ( 0.000017 0.000014 0.000012 ) 0.072508 -0.029252 0.033014 ( 0.000012 0.000010 0.000008 ) -0.036256 -0.003632 0.076506 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007194 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000007 -0.000010 0.007184 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3616(11) 8.3625(14) 8.3688(11) 89.917(12) 90.058(11) 89.978(12) V = 585.18(15) OTKP changes: 479 1 1 1 OTKP changes: 479 1 1 1 OTKP changes: 479 1 1 1 No constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007208 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007205 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007196 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 479 obs out of 481 (total:481,skipped:0) (99.58%) unit cell: 8.3548(11) 8.3562(14) 8.3616(11) 89.936(12) 90.003(11) 89.960(12) V = 583.76(15) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.749) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007208 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007205 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007196 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 479 obs out of 481 (total:481,skipped:0) (99.58%) unit cell: 8.3548(11) 8.3562(14) 8.3616(11) 89.936(12) 90.003(11) 89.960(12) V = 583.76(15) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 479 obs out of 481 (total:481,skipped:0) (99.58%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007208 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007205 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007196 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025023 -0.079587 -0.015471 ( 0.000016 0.000014 0.000012 ) 0.072556 -0.029299 0.032986 ( 0.000011 0.000010 0.000008 ) -0.036292 -0.003563 0.076605 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 479 obs out of 481 (total:481,skipped:0) (99.58%) unit cell: 8.3548(11) 8.3562(14) 8.3616(11) 89.936(12) 90.003(11) 89.960(12) V = 583.76(15) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025008 -0.079543 -0.015716 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029338 0.032914 ( 0.000009 0.000014 0.000014 ) -0.036185 -0.003657 0.076521 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007179 -0.000003 0.000008 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007201 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000008 0.000005 0.007186 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3711(11) 8.3585(12) 8.3675(11) 90.037(11) 90.062(11) 89.975(11) V = 585.47(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007190 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007208 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007202 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3648(10) 8.3546(12) 8.3581(11) 89.998(11) 90.022(10) 90.029(11) V = 584.10(13) unit cell: 8.3592(3) 8.3592(3) 8.3592(3) 90.0 90.0 90.0 V = 584.10(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.749) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007190 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007208 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007202 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3648(10) 8.3546(12) 8.3581(11) 89.998(11) 90.022(10) 90.029(11) V = 584.10(13) unit cell: 8.3592(3) 8.3592(3) 8.3592(3) 90.0 90.0 90.0 V = 584.10(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007190 0.000004 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000004 0.007208 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007202 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025086 -0.079571 -0.015731 ( 0.000008 0.000013 0.000013 ) 0.072405 -0.029372 0.032995 ( 0.000008 0.000014 0.000013 ) -0.036310 -0.003694 0.076588 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3648(10) 8.3546(12) 8.3581(11) 89.998(11) 90.022(10) 90.029(11) V = 584.10(13) unit cell: 8.3592(3) 8.3592(3) 8.3592(3) 90.0 90.0 90.0 V = 584.10(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025235 -0.079453 -0.015776 ( 0.000011 0.000016 0.000017 ) 0.072348 -0.029412 0.032795 ( 0.000008 0.000011 0.000012 ) -0.036273 -0.003614 0.076597 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007187 0.000008 -0.000008 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000012 ( 0.000001 0.000003 0.000002 ) -0.000008 0.000012 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3669(10) 8.3645(14) 8.3642(11) 90.096(13) 89.939(10) 90.065(12) V = 585.36(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007199 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3589(10) 8.3598(14) 8.3555(11) 90.051(12) 89.993(10) 90.064(12) V = 583.87(14) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.87(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.749) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007199 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3589(10) 8.3598(14) 8.3555(11) 90.051(12) 89.993(10) 90.064(12) V = 583.87(14) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007199 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025253 -0.079499 -0.015751 ( 0.000011 0.000015 0.000017 ) 0.072473 -0.029418 0.032808 ( 0.000008 0.000011 0.000012 ) -0.036199 -0.003659 0.076693 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3589(10) 8.3598(14) 8.3555(11) 90.051(12) 89.993(10) 90.064(12) V = 583.87(14) unit cell: 8.3581(3) 8.3581(3) 8.3581(3) 90.0 90.0 90.0 V = 583.87(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 OTKP changes: 472 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) unit cell: 8.3674(3) 8.3674(3) 8.3674(3) 90.0 90.0 90.0 V = 585.82(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079378 -0.015694 ( 0.000011 0.000008 0.000010 ) 0.072398 -0.029480 0.032786 ( 0.000014 0.000011 0.000014 ) -0.036094 -0.003538 0.076607 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3676(13) 8.3694(9) 8.3651(12) 90.065(10) 90.048(12) 90.028(10) V = 585.82(14) unit cell: 8.3674(3) 8.3674(3) 8.3674(3) 90.0 90.0 90.0 V = 585.82(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 94 obs out of 94 (total:94,skipped:0) (100.00%) UB - matrix: -0.025096 -0.079428 -0.015772 ( 0.000079 0.000071 0.000063 ) 0.072324 -0.029570 0.032779 ( 0.000064 0.000058 0.000051 ) -0.036302 -0.003281 0.076566 ( 0.000073 0.000066 0.000058 ) M - matrix: 0.007178 -0.000026 -0.000013 ( 0.000011 0.000008 0.000008 ) -0.000026 0.007194 0.000032 ( 0.000008 0.000012 0.000008 ) -0.000013 0.000032 0.007186 ( 0.000008 0.000008 0.000010 ) unit cell: 8.372(6) 8.363(7) 8.368(6) 90.26(6) 89.90(6) 89.79(6) V = 585.8(8) OTKP changes: 94 1 1 1 No constraint UB - matrix: -0.025073 -0.079452 -0.015754 ( 0.000077 0.000069 0.000061 ) 0.072435 -0.029619 0.032795 ( 0.000062 0.000056 0.000050 ) -0.036336 -0.003346 0.076682 ( 0.000074 0.000066 0.000059 ) M - matrix: 0.007196 -0.000032 -0.000016 ( 0.000011 0.000008 0.000008 ) -0.000032 0.007201 0.000024 ( 0.000008 0.000011 0.000007 ) -0.000016 0.000024 0.007204 ( 0.000008 0.000007 0.000010 ) Constraint UB - matrix: -0.025073 -0.079452 -0.015754 ( 0.000077 0.000069 0.000061 ) 0.072435 -0.029619 0.032795 ( 0.000062 0.000056 0.000050 ) -0.036336 -0.003346 0.076682 ( 0.000074 0.000066 0.000059 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 94 obs out of 94 (total:94,skipped:0) (100.00%) unit cell: 8.362(6) 8.359(7) 8.357(6) 90.19(6) 89.88(6) 89.75(6) V = 584.1(8) unit cell: 8.3591(8) 8.3591(8) 8.3591(8) 90.0 90.0 90.0 V = 584.09(10) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.860) HKL list info: 258 refl (0 shortened) PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.025073 -0.079452 -0.015754 ( 0.000077 0.000069 0.000061 ) 0.072435 -0.029619 0.032795 ( 0.000062 0.000056 0.000050 ) -0.036336 -0.003346 0.076682 ( 0.000074 0.000066 0.000059 ) M - matrix: 0.007196 -0.000032 -0.000016 ( 0.000011 0.000008 0.000008 ) -0.000032 0.007201 0.000024 ( 0.000008 0.000011 0.000007 ) -0.000016 0.000024 0.007204 ( 0.000008 0.000007 0.000010 ) Constraint UB - matrix: -0.025073 -0.079452 -0.015754 ( 0.000077 0.000069 0.000061 ) 0.072435 -0.029619 0.032795 ( 0.000062 0.000056 0.000050 ) -0.036336 -0.003346 0.076682 ( 0.000074 0.000066 0.000059 ) M - matrix: 0.007177 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007177 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007177 ( 0.000000 0.000000 0.000001 ) UB fit with 94 obs out of 94 (total:94,skipped:0) (100.00%) unit cell: 8.362(6) 8.359(7) 8.357(6) 90.19(6) 89.88(6) 89.75(6) V = 584.1(8) unit cell: 8.3591(8) 8.3591(8) 8.3591(8) 90.0 90.0 90.0 V = 584.09(10) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025040 -0.079425 -0.015586 ( 0.000006 0.000006 0.000006 ) 0.072500 -0.029226 0.032903 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003574 0.076545 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 -0.000001 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007185 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025040 -0.079425 -0.015586 ( 0.000006 0.000006 0.000006 ) 0.072500 -0.029226 0.032903 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003574 0.076545 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) UB fit with 2812 obs out of 2817 (total:2817,skipped:0) (99.82%) unit cell: 8.3620(6) 8.3736(6) 8.3682(5) 90.022(5) 90.026(5) 89.995(6) V = 585.94(7) unit cell: 8.36792(19) 8.36792(19) 8.36792(19) 90.0 90.0 90.0 V = 585.94(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region 23 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof 3826 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:12:06 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.749) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.749) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.749) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.860) PROFFIT INFO: signal sum: min=142.0000 max=23168420.0000 PROFFIT INFO: signal sum lp corr: min=218.9709 max=3210474.8652 PROFFIT INFO: background sum: min=612.0000 max=26038.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11900.0000 PROFFIT INFO: num of signal pixels: min=51 max=501 PROFFIT INFO: Inet: min=350.3535 max=5136759.5000 PROFFIT INFO: sig(Inet): min=120.2283 max=47799.8672 PROFFIT INFO: Inet/sig(Inet): min=0.38 max=248.46 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 46 190 413 782 881 1603 2563 3514 3826 Percent 0.0 0.1 1.2 5.0 10.8 20.4 23.0 41.9 67.0 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3826 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3826 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5136760- 1120384 382 1858341.82 121.45 100.00 1119844- 615554 382 837581.59 102.06 100.00 615472- 259814 382 405129.60 94.04 100.00 259696- 167329 382 199791.02 71.33 100.00 166962- 117711 382 141842.13 50.17 100.00 117661- 89485 382 102838.67 35.34 100.00 89381- 63539 382 77719.60 28.61 100.00 63474- 5319 382 35084.81 18.60 100.00 5308- 2883 382 3816.40 5.23 96.60 2882- 350 388 2075.14 3.68 54.38 ------------------------------------------------------------------------------------ 5136760- 350 3826 365850.70 52.97 95.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 757879.29 92.58 100.00 1.41- 1.12 382 596962.18 63.19 99.48 1.12- 0.96 382 504000.89 70.79 97.38 0.96- 0.88 382 343905.30 59.27 94.50 0.88- 0.81 382 443114.22 68.19 99.48 0.81- 0.73 382 241812.69 40.94 95.29 0.73- 0.71 382 173634.38 34.34 89.27 0.71- 0.65 382 306095.55 46.87 93.72 0.65- 0.62 382 149057.89 26.91 87.43 0.62- 0.58 388 145505.56 27.06 93.81 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 365850.70 52.97 95.03 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:12:06 2018 Sorting 3826 observations 120 unique observations with > 7.00 F2/sig(F2) 3826 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 24 653 Total number of frames 653 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3826 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 4 112 Total number of frames 112 3068 observations > 7.00 F2/sig(F2) 3068 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 4 112 Total number of frames 112 Removing 'redundancy=1' reflections Average redundancy: 23.6 (Out of 3068 removed 3 = 3065, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3065 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 4 112 Total number of frames 112 130 unique data precomputed (should be 130) 130 unique data with 3065 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 23.6 (Out of 3065 removed 0 = 3065, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3065 observations RMS deviation of equivalent data = 0.25337 Rint = 0.18717 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18155, wR= 0.26316 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14031, wR= 0.18468, Acormin=0.609, Acormax=1.370, Acor_av=0.994 F test: Probability=1.000, F= 1.671 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12515, wR= 0.15898, Acormin=0.537, Acormax=1.434, Acor_av=0.907 F test: Probability=1.000, F= 1.256 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11588, wR= 0.15812, Acormin=0.639, Acormax=1.613, Acor_av=0.982 F test: Probability=1.000, F= 1.164 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09814, wR= 0.13259, Acormin=0.493, Acormax=1.555, Acor_av=0.894 F test: Probability=1.000, F= 1.393 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08767, wR= 0.12121, Acormin=0.477, Acormax=1.605, Acor_av=0.905 F test: Probability=1.000, F= 1.250 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10609, wR= 0.14716, Acormin=0.650, Acormax=1.681, Acor_av=0.986 F test: Probability=0.000, F= 0.682 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09003, wR= 0.12448, Acormin=0.495, Acormax=1.648, Acor_av=0.904 F test: Probability=0.000, F= 0.946 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08216, wR= 0.11573, Acormin=0.479, Acormax=1.650, Acor_av=0.911 F test: Probability=1.000, F= 1.134 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07835, wR= 0.10859, Acormin=0.350, Acormax=1.518, Acor_av=0.861 F test: Probability=0.993, F= 1.096 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10905, wR= 0.14216, Acormin=0.451, Acormax=1.459, Acor_av=0.835 F test: Probability=0.000, F= 0.517 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08879, wR= 0.11973, Acormin=0.484, Acormax=1.612, Acor_av=0.892 F test: Probability=0.000, F= 0.779 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08864, wR= 0.11773, Acormin=0.098, Acormax=0.373, Acor_av=0.204 F test: Probability=0.000, F= 0.780 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07989, wR= 0.10827, Acormin=0.097, Acormax=0.398, Acor_av=0.227 F test: Probability=0.000, F= 0.956 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07433, wR= 0.10095, Acormin=0.104, Acormax=0.432, Acor_av=0.238 F test: Probability=0.994, F= 1.099 Final absorption model (ne=6, no=5): Rint= 0.07835, Acormin=0.350, Acormax=1.518, Acor_av=0.861 Combined refinement in use Rint: 0.18729 There are 112 active scales (one needs to be fixed) Refinement control: frame scale #110 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 159 pars with 12720 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25337 Using Levenberg-Marquardt: 0.00010 New wR= 0.06638 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18717 with corrections 0.05191 Rint for all data: 0.18729 with corrections 0.05214 0 observations identified as outliers and rejected Cycle 2 wR= 0.06638 Using Levenberg-Marquardt: 0.00001 New wR= 0.06241 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18717 with corrections 0.04882 Rint for all data: 0.18729 with corrections 0.04905 0 observations identified as outliers and rejected Cycle 3 wR= 0.06241 Using Levenberg-Marquardt: 0.00000 New wR= 0.06142 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18717 with corrections 0.04810 Rint for all data: 0.18729 with corrections 0.04833 0 observations identified as outliers and rejected Cycle 4 wR= 0.06142 Using Levenberg-Marquardt: 0.00000 New wR= 0.06086 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18717 with corrections 0.04765 Rint for all data: 0.18729 with corrections 0.04788 0 observations identified as outliers and rejected Cycle 5 wR= 0.06086 Using Levenberg-Marquardt: 0.00000 New wR= 0.06048 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18717 with corrections 0.04735 Rint for all data: 0.18729 with corrections 0.04758 0 observations identified as outliers and rejected Final wR= 0.06048 Final frame scales: Min= 0.7785 Max= 1.3411 Final absorption correction factors: Amin= 0.4925 Amax= 1.5429 PROFFIT INFO: Inet (after scale3 abspack): min=695.7189 max=4576736.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=141.6265 max=52087.0625 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 3826 reflections read from tmp file 821 reflections are rejected (821 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 5 4 4 5 1 4 4 127 Initial Chi^2= 0.44614 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.82292 Current error model SIG(F2)^2 = 140.12*I_RAW + 0.00*I_BACK+(0.02560*)^2 Cycle 2, Chi^2= 1.00065 Current error model SIG(F2)^2 = 123.92*I_RAW + 0.00*I_BACK+(0.02127*)^2 Cycle 3, Chi^2= 0.99997 Current error model SIG(F2)^2 = 122.83*I_RAW + 0.00*I_BACK+(0.02153*)^2 Cycle 4, Chi^2= 1.00001 Current error model SIG(F2)^2 = 123.02*I_RAW + 0.00*I_BACK+(0.02149*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 123.02*I_RAW + 0.00*I_BACK+(0.02149*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4576737- 1074837 382 1746602.72 43.33 100.00 1071531- 593728 382 796827.87 36.36 100.00 593562- 251958 382 393082.19 34.98 100.00 251950- 150881 382 188026.51 30.57 100.00 150834- 120885 382 136220.80 24.62 100.00 120851- 85513 382 99022.75 18.82 100.00 85503- 66414 382 76209.38 16.17 100.00 66373- 4794 382 37408.89 11.48 100.00 4748- 2717 382 3534.02 4.47 93.98 2705- 696 388 2091.34 3.63 70.10 ------------------------------------------------------------------------------------ 4576737- 696 3826 347360.34 22.41 96.37 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 754816.65 35.31 100.00 1.41- 1.12 382 574108.95 27.73 99.21 1.12- 0.96 382 462002.90 26.83 97.91 0.96- 0.88 382 321929.79 23.04 96.34 0.88- 0.81 382 418318.63 26.34 99.48 0.81- 0.73 382 220744.73 18.26 96.07 0.73- 0.71 382 164986.95 17.01 91.10 0.71- 0.65 382 287002.14 21.46 97.38 0.65- 0.62 382 139287.11 13.96 90.58 0.62- 0.58 388 133760.51 14.32 95.62 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 347360.34 22.41 96.37 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 754816.65 35.31 100.00 4.82- 1.12 764 664462.80 31.52 99.61 4.82- 0.96 1146 596976.17 29.96 99.04 4.82- 0.88 1528 528214.58 28.23 98.36 4.82- 0.81 1910 506235.39 27.85 98.59 4.82- 0.73 2292 458653.61 26.25 98.17 4.82- 0.71 2674 416701.23 24.93 97.16 4.82- 0.65 3056 400488.84 24.50 97.19 4.82- 0.62 3438 371466.43 23.33 96.45 4.82- 0.58 3826 347360.34 22.41 96.37 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 347360.34 22.41 96.37 Scale applied to data: s=0.218496 (maximum obs:4576736.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.029: data 3826 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.029: data 3813 -> merged 157 Rejected total: 13, method kkm 9, method Blessing 4 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585871, 4.831220 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 22.29 100.00 312 1.41 - 1.12 14 14 31.43 100.00 440 1.12 - 0.97 14 14 31.50 100.00 441 0.96 - 0.84 14 14 33.29 100.00 466 0.84 - 0.78 14 14 25.71 100.00 360 0.78 - 0.73 14 14 26.86 100.00 376 0.73 - 0.69 14 14 25.00 100.00 350 0.69 - 0.66 14 14 21.43 100.00 300 0.65 - 0.63 14 14 22.29 100.00 312 0.63 - 0.60 14 14 19.64 100.00 275 --------------------------------------------------------------- 8.36 - 0.60 140 140 25.94 100.00 3632 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:12:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361994 8.373613 8.368152 90.0218 90.0263 89.9947 3813 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1946 0 2555 2555 3813 N (int>3sigma) = 0 0 0 0 1946 0 2465 2457 3674 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.9 78.2 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.2 0.0 22.4 22.6 22.4 Lattice type: F chosen Volume: 585.94 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.914 5.916 5.917 119.96 119.97 90.04 Niggli form: a.a = 34.971 b.b = 35.003 c.c = 35.007 b.c = -17.480 a.c = -17.478 a.b = -0.026 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.044 CUBIC F-lattice R(int) = 0.047 [ 3656] Vol = 585.9 Cell: 8.374 8.368 8.362 89.97 90.01 90.02 Volume: 585.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.049 TETRAGONAL I-lattice R(int) = 0.046 [ 3405] Vol = 293.0 Cell: 5.920 5.918 8.362 90.01 89.98 89.96 Volume: 292.97 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.042 TETRAGONAL I-lattice R(int) = 0.046 [ 3400] Vol = 293.0 Cell: 5.914 5.916 8.374 89.98 90.01 90.04 Volume: 292.97 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.023 TETRAGONAL I-lattice R(int) = 0.046 [ 3405] Vol = 293.0 Cell: 5.918 5.920 8.362 90.02 90.01 90.04 Volume: 292.97 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.034 ORTHORHOMBIC F-lattice R(int) = 0.046 [ 3363] Vol = 585.9 Cell: 8.362 8.368 8.374 90.02 90.01 89.97 Volume: 585.94 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.053 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3351] Vol = 293.0 Cell: 8.362 5.918 5.920 89.96 89.98 90.01 Volume: 292.97 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.034 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 3348] Vol = 293.0 Cell: 5.914 5.916 8.374 90.02 89.99 90.04 Volume: 292.97 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 3016] Vol = 293.0 Cell: 5.918 8.362 5.920 90.02 90.04 90.01 Volume: 292.97 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.034 MONOCLINIC I-lattice R(int) = 0.044 [ 3012] Vol = 293.0 Cell: 5.917 8.368 5.917 89.97 90.08 90.00 Volume: 292.97 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 3016] Vol = 293.0 Cell: 5.918 8.362 5.920 90.02 90.04 90.01 Volume: 292.97 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.027 MONOCLINIC I-lattice R(int) = 0.044 [ 2998] Vol = 293.0 Cell: 5.916 5.914 8.374 90.01 90.02 89.96 Volume: 292.97 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.010 MONOCLINIC I-lattice R(int) = 0.045 [ 3010] Vol = 293.0 Cell: 5.914 8.374 5.916 89.98 90.04 90.01 Volume: 292.97 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.013 MONOCLINIC I-lattice R(int) = 0.045 [ 3010] Vol = 293.0 Cell: 5.914 8.374 5.916 90.02 90.04 89.99 Volume: 292.97 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2322] Vol = 146.5 Cell: 5.914 5.916 5.917 119.96 119.97 90.04 Volume: 146.48 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1946 0 2548 2555 3813 N (int>3sigma) = 0 0 0 0 1946 0 2453 2457 3674 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.6 78.2 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.2 0.0 22.4 22.6 22.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 286 855 N I>3s 38 38 270 855 0.9 0.9 0.7 35.6 8.3 8.3 5.2 25.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3390 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3429 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.373613 8.368152 8.361994 89.9737 90.0053 90.0218 ZERR 3.00 0.000624 0.000487 0.000594 0.0053 0.0059 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3913504- 730988 625 624 26 24.0 1406224.25 41.06 0.041 0.056 724831- 220601 588 585 26 22.5 439849.63 35.01 0.061 0.076 215325- 95232 887 887 26 34.1 145097.94 25.36 0.045 0.058 91880- 65178 628 626 26 24.1 79864.04 16.38 0.071 0.090 62067- 3486 479 475 26 18.3 24146.23 8.59 0.088 0.120 3327- 1689 619 616 27 22.8 2608.21 4.12 0.201 0.265 ------------------------------------------------------------------------------------------- 3913504- 1689 3826 3813 157 24.3 347906.86 22.42 0.047 0.063 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 716 710 26 27.3 609862.19 30.79 0.046 0.063 0.024 1.12-0.88 844 842 26 32.4 449857.64 26.11 0.035 0.047 0.026 0.85-0.75 709 709 26 27.3 317737.22 21.82 0.044 0.054 0.030 0.74-0.68 621 620 26 23.8 254072.70 19.74 0.060 0.072 0.034 0.67-0.63 588 587 26 22.6 142897.02 15.40 0.076 0.093 0.043 0.62-0.59 348 345 27 12.8 139435.48 14.11 0.077 0.078 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 3826 3813 157 24.3 347906.86 22.42 0.047 0.063 0.029 inf-0.60 3641 3630 139 26.1 360234.55 22.89 0.047 0.062 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 710 26 26 100.0 27.3 609862.19 174.62 0.046 0.006 1.12-0.88 842 26 26 100.0 32.4 449857.64 151.47 0.035 0.005 0.85-0.75 709 26 26 100.0 27.3 317737.22 120.69 0.044 0.006 0.74-0.68 620 26 26 100.0 23.8 254072.70 98.61 0.060 0.008 0.67-0.63 587 26 26 100.0 22.6 142897.02 72.47 0.076 0.009 0.62-0.59 345 27 27 100.0 12.8 139435.48 57.38 0.077 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3813 157 157 100.0 24.3 347906.86 120.79 0.047 0.007 inf-0.60 3630 139 139 100.0 26.1 360234.55 124.49 0.047 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025040 -0.079424 -0.015586 ( 0.000006 0.000006 0.000006 ) 0.072501 -0.029226 0.032903 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003574 0.076545 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 -0.000001 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007185 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025040 -0.079424 -0.015586 ( 0.000006 0.000006 0.000006 ) 0.072501 -0.029226 0.032903 ( 0.000006 0.000007 0.000007 ) -0.036220 -0.003574 0.076545 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007184 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007184 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007184 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3620(6) 8.3737(6) 8.3682(5) 90.022(5) 90.026(5) 89.995(6) V = 585.94(7) unit cell: 8.36793(19) 8.36793(19) 8.36793(19) 90.0 90.0 90.0 V = 585.94(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.749) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.749) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.749) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) Run 7 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.860) PROFFIT INFO: signal sum: min=142.0000 max=23168420.0000 PROFFIT INFO: signal sum lp corr: min=218.9709 max=3210474.8652 PROFFIT INFO: background sum: min=612.0000 max=26038.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11900.0000 PROFFIT INFO: num of signal pixels: min=51 max=501 PROFFIT INFO: Inet: min=350.3535 max=5136759.5000 PROFFIT INFO: sig(Inet): min=120.2283 max=47799.8672 PROFFIT INFO: Inet/sig(Inet): min=0.38 max=248.46 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 92 380 826 1564 1762 3206 5126 7028 7652 Percent 0.0 0.1 1.2 5.0 10.8 20.4 23.0 41.9 67.0 91.8 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3826 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3826 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5136760- 1120384 382 1858341.82 121.45 100.00 1119844- 615554 382 837581.59 102.06 100.00 615472- 259814 382 405129.60 94.04 100.00 259696- 167329 382 199791.02 71.33 100.00 166962- 117711 382 141842.13 50.17 100.00 117661- 89485 382 102838.67 35.34 100.00 89381- 63539 382 77719.60 28.61 100.00 63474- 5319 382 35084.81 18.60 100.00 5308- 2883 382 3816.40 5.23 96.60 2882- 350 388 2075.14 3.68 54.38 ------------------------------------------------------------------------------------ 5136760- 350 3826 365850.70 52.97 95.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 757879.29 92.58 100.00 1.41- 1.12 382 596962.18 63.19 99.48 1.12- 0.96 382 504000.89 70.79 97.38 0.96- 0.88 382 343905.30 59.27 94.50 0.88- 0.81 382 443114.22 68.19 99.48 0.81- 0.73 382 241812.69 40.94 95.29 0.73- 0.71 382 173634.38 34.34 89.27 0.71- 0.65 382 306095.55 46.87 93.72 0.65- 0.62 382 149057.89 26.91 87.43 0.62- 0.58 388 145505.56 27.06 93.81 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 365850.70 52.97 95.03 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:12:08 2018 Sorting 3826 observations 86 unique observations with > 7.00 F2/sig(F2) 3826 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 24 653 Total number of frames 653 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3826 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 3 86 Total number of frames 86 3068 observations > 7.00 F2/sig(F2) 3068 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 3 86 Total number of frames 86 Removing 'redundancy=1' reflections Average redundancy: 33.0 (Out of 3068 removed 3 = 3065, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3065 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 3 86 Total number of frames 86 93 unique data precomputed (should be 93) 93 unique data with 3065 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 33.0 (Out of 3065 removed 0 = 3065, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3065 observations RMS deviation of equivalent data = 0.25380 Rint = 0.18743 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.18174, wR= 0.26211 Trying model 1 (ne=2, no=0)... Results: Rint= 0.14037, wR= 0.18452, Acormin=0.610, Acormax=1.368, Acor_av=0.994 F test: Probability=1.000, F= 1.673 Trying model 2 (ne=2, no=1)... Results: Rint= 0.12531, wR= 0.15916, Acormin=0.539, Acormax=1.431, Acor_av=0.907 F test: Probability=1.000, F= 1.254 Trying model 3 (ne=4, no=0)... Results: Rint= 0.11583, wR= 0.15806, Acormin=0.639, Acormax=1.609, Acor_av=0.982 F test: Probability=1.000, F= 1.168 Trying model 4 (ne=4, no=1)... Results: Rint= 0.09796, wR= 0.13278, Acormin=0.495, Acormax=1.549, Acor_av=0.894 F test: Probability=1.000, F= 1.397 Trying model 5 (ne=4, no=3)... Results: Rint= 0.08758, wR= 0.12152, Acormin=0.477, Acormax=1.602, Acor_av=0.905 F test: Probability=1.000, F= 1.248 Trying model 6 (ne=6, no=0)... Results: Rint= 0.10578, wR= 0.14698, Acormin=0.652, Acormax=1.677, Acor_av=0.989 F test: Probability=0.000, F= 0.685 Trying model 7 (ne=6, no=1)... Results: Rint= 0.08998, wR= 0.12450, Acormin=0.500, Acormax=1.637, Acor_av=0.906 F test: Probability=0.000, F= 0.945 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08192, wR= 0.11579, Acormin=0.483, Acormax=1.654, Acor_av=0.912 F test: Probability=1.000, F= 1.138 Trying model 9 (ne=6, no=5)... Results: Rint= 0.07835, wR= 0.10871, Acormin=0.358, Acormax=1.518, Acor_av=0.864 F test: Probability=0.989, F= 1.089 Trying model 10 (ne=8, no=0)... Results: Rint= 0.10899, wR= 0.14183, Acormin=0.458, Acormax=1.450, Acor_av=0.838 F test: Probability=0.000, F= 0.517 Trying model 11 (ne=8, no=1)... Results: Rint= 0.08862, wR= 0.11948, Acormin=0.491, Acormax=1.617, Acor_av=0.894 F test: Probability=0.000, F= 0.782 Trying model 12 (ne=8, no=3)... Results: Rint= 0.08837, wR= 0.11757, Acormin=0.100, Acormax=0.376, Acor_av=0.205 F test: Probability=0.000, F= 0.784 Trying model 13 (ne=8, no=5)... Results: Rint= 0.07980, wR= 0.10826, Acormin=0.100, Acormax=0.401, Acor_av=0.228 F test: Probability=0.000, F= 0.958 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07418, wR= 0.10100, Acormin=0.105, Acormax=0.434, Acor_av=0.239 F test: Probability=0.996, F= 1.103 Final absorption model (ne=6, no=5): Rint= 0.07835, Acormin=0.358, Acormax=1.518, Acor_av=0.864 Combined refinement in use Rint: 0.18754 There are 86 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 133 pars with 8911 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25380 Using Levenberg-Marquardt: 0.00010 New wR= 0.06729 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18743 with corrections 0.05275 Rint for all data: 0.18754 with corrections 0.05298 0 observations identified as outliers and rejected Cycle 2 wR= 0.06729 Using Levenberg-Marquardt: 0.00001 New wR= 0.06228 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18743 with corrections 0.04905 Rint for all data: 0.18754 with corrections 0.04927 0 observations identified as outliers and rejected Cycle 3 wR= 0.06228 Using Levenberg-Marquardt: 0.00000 New wR= 0.06093 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18743 with corrections 0.04811 Rint for all data: 0.18754 with corrections 0.04834 0 observations identified as outliers and rejected Cycle 4 wR= 0.06093 Using Levenberg-Marquardt: 0.00000 New wR= 0.06029 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18743 with corrections 0.04761 Rint for all data: 0.18754 with corrections 0.04784 0 observations identified as outliers and rejected Cycle 5 wR= 0.06029 Using Levenberg-Marquardt: 0.00000 New wR= 0.05994 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.18743 with corrections 0.04728 Rint for all data: 0.18754 with corrections 0.04751 0 observations identified as outliers and rejected Final wR= 0.05994 Final frame scales: Min= 0.7273 Max= 1.2220 Final absorption correction factors: Amin= 0.4861 Amax= 1.4193 PROFFIT INFO: Inet (after scale3 abspack): min=676.2575 max=4545349.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=140.7361 max=52796.6367 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 3826 reflections read from tmp file 820 reflections are rejected (820 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 2 5 2 1 1 3 4 91 Initial Chi^2= 0.40826 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88239 Current error model SIG(F2)^2 = 138.50*I_RAW + 0.00*I_BACK+(0.02165*)^2 Cycle 2, Chi^2= 1.00056 Current error model SIG(F2)^2 = 111.38*I_RAW + 0.00*I_BACK+(0.02239*)^2 Cycle 3, Chi^2= 1.00010 Current error model SIG(F2)^2 = 113.69*I_RAW + 0.00*I_BACK+(0.02193*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 113.28*I_RAW + 0.00*I_BACK+(0.02202*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 113.36*I_RAW + 0.00*I_BACK+(0.02200*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 113.36*I_RAW + 0.00*I_BACK+(0.02200*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4545350- 1076038 382 1748646.66 42.71 100.00 1070401- 592161 382 796448.83 36.39 100.00 589681- 253041 382 393403.10 34.98 100.00 251540- 150975 382 188201.15 30.93 100.00 150856- 120895 382 136222.35 25.11 100.00 120730- 85389 382 98752.10 19.33 100.00 85386- 66426 382 76261.19 16.75 100.00 66398- 4795 382 37518.88 11.85 100.00 4788- 2704 382 3534.90 4.64 97.12 2703- 676 388 2094.02 3.79 74.74 ------------------------------------------------------------------------------------ 4545350- 676 3826 347565.69 22.62 97.15 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 755346.05 35.08 100.00 1.41- 1.12 382 575560.96 27.73 99.48 1.12- 0.96 382 461833.45 26.93 98.17 0.96- 0.88 382 322273.85 23.27 97.38 0.88- 0.81 382 418392.79 26.57 99.74 0.81- 0.73 382 221103.21 18.54 96.86 0.73- 0.71 382 164872.07 17.39 92.41 0.71- 0.65 382 286391.57 21.81 98.17 0.65- 0.62 382 139585.89 14.30 92.41 0.62- 0.58 388 133656.91 14.69 96.91 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 347565.69 22.62 97.15 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 382 755346.05 35.08 100.00 4.82- 1.12 764 665453.51 31.41 99.74 4.82- 0.96 1146 597580.15 29.92 99.21 4.82- 0.88 1528 528753.58 28.25 98.76 4.82- 0.81 1910 506681.42 27.92 98.95 4.82- 0.73 2292 459085.05 26.35 98.60 4.82- 0.71 2674 417054.63 25.07 97.72 4.82- 0.65 3056 400721.74 24.67 97.77 4.82- 0.62 3438 371706.65 23.51 97.18 4.82- 0.58 3826 347565.69 22.62 97.15 ------------------------------------------------------------------------------------ 4.82- 0.58 3826 347565.69 22.62 97.15 Scale applied to data: s=0.220005 (maximum obs:4545349.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.029: data 3826 -> merged 110 With outlier rejection... Rint 0.047; Rsigma 0.029: data 3811 -> merged 110 Rejected total: 15, method kkm 11, method Blessing 4 Completeness direct cell (a, b, c) = (8.368, 8.368, 8.368), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585873, 4.831229 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 24.00 100.00 240 1.61 - 1.21 10 10 35.10 100.00 351 1.17 - 1.01 10 10 45.40 100.00 454 0.99 - 0.89 10 10 44.10 100.00 441 0.88 - 0.81 10 10 42.30 100.00 423 0.81 - 0.74 10 10 36.80 100.00 368 0.73 - 0.71 10 10 40.30 100.00 403 0.70 - 0.66 10 10 33.70 100.00 337 0.66 - 0.64 10 10 31.60 100.00 316 0.63 - 0.60 10 10 29.70 100.00 297 --------------------------------------------------------------- 8.36 - 0.60 100 100 36.30 100.00 3630 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:12:07 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361994 8.373613 8.368152 90.0218 90.0263 89.9947 3813 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.42 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1946 0 2555 2555 3813 N (int>3sigma) = 0 0 0 0 1946 0 2465 2457 3674 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.9 78.2 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.2 0.0 22.4 22.6 22.4 Lattice type: F chosen Volume: 585.94 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.914 5.916 5.917 119.96 119.97 90.04 Niggli form: a.a = 34.971 b.b = 35.003 c.c = 35.007 b.c = -17.480 a.c = -17.478 a.b = -0.026 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.044 CUBIC F-lattice R(int) = 0.047 [ 3656] Vol = 585.9 Cell: 8.374 8.368 8.362 89.97 90.01 90.02 Volume: 585.94 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.049 TETRAGONAL I-lattice R(int) = 0.046 [ 3405] Vol = 293.0 Cell: 5.920 5.918 8.362 90.01 89.98 89.96 Volume: 292.97 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.042 TETRAGONAL I-lattice R(int) = 0.046 [ 3400] Vol = 293.0 Cell: 5.914 5.916 8.374 89.98 90.01 90.04 Volume: 292.97 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.023 TETRAGONAL I-lattice R(int) = 0.046 [ 3405] Vol = 293.0 Cell: 5.918 5.920 8.362 90.02 90.01 90.04 Volume: 292.97 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.034 ORTHORHOMBIC F-lattice R(int) = 0.046 [ 3363] Vol = 585.9 Cell: 8.362 8.368 8.374 90.02 90.01 89.97 Volume: 585.94 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.053 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3351] Vol = 293.0 Cell: 8.362 5.918 5.920 89.96 89.98 90.01 Volume: 292.97 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.034 ORTHORHOMBIC I-lattice R(int) = 0.045 [ 3348] Vol = 293.0 Cell: 5.914 5.916 8.374 90.02 89.99 90.04 Volume: 292.97 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 3016] Vol = 293.0 Cell: 5.918 8.362 5.920 90.02 90.04 90.01 Volume: 292.97 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.034 MONOCLINIC I-lattice R(int) = 0.044 [ 3012] Vol = 293.0 Cell: 5.917 8.368 5.917 89.97 90.08 90.00 Volume: 292.97 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.033 MONOCLINIC I-lattice R(int) = 0.043 [ 3016] Vol = 293.0 Cell: 5.918 8.362 5.920 90.02 90.04 90.01 Volume: 292.97 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.027 MONOCLINIC I-lattice R(int) = 0.044 [ 2998] Vol = 293.0 Cell: 5.916 5.914 8.374 90.01 90.02 89.96 Volume: 292.97 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.010 MONOCLINIC I-lattice R(int) = 0.045 [ 3010] Vol = 293.0 Cell: 5.914 8.374 5.916 89.98 90.04 90.01 Volume: 292.97 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.013 MONOCLINIC I-lattice R(int) = 0.045 [ 3010] Vol = 293.0 Cell: 5.914 8.374 5.916 90.02 90.04 89.99 Volume: 292.97 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2322] Vol = 146.5 Cell: 5.914 5.916 5.917 119.96 119.97 90.04 Volume: 146.48 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 1946 0 2548 2555 3813 N (int>3sigma) = 0 0 0 0 1946 0 2453 2457 3674 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.6 78.2 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.2 0.0 22.4 22.6 22.4 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.180 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 38 38 286 855 N I>3s 38 38 270 855 0.9 0.9 0.7 35.6 8.3 8.3 5.2 25.8 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3390 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3429 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.373613 8.368152 8.361994 89.9737 90.0053 90.0218 ZERR 3.00 0.000624 0.000487 0.000594 0.0053 0.0059 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3929177- 498355 849 847 27 31.4 1201295.89 38.76 0.045 0.060 489563- 117377 1125 1122 27 41.6 208561.89 29.82 0.050 0.063 103292- 34790 948 946 27 35.0 76725.70 16.74 0.067 0.086 10205- 1795 904 896 29 30.9 3401.92 4.58 0.167 0.212 ------------------------------------------------------------------------------------------- 3929177- 1795 3826 3811 110 34.6 348237.92 22.63 0.047 0.062 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 971 965 27 35.7 629845.86 31.56 0.044 0.062 0.024 1.01-0.78 1174 1171 28 41.8 318795.45 21.87 0.039 0.047 0.029 0.76-0.65 1010 1009 28 36.0 240295.03 19.29 0.055 0.068 0.034 0.65-0.59 671 666 27 24.7 155504.94 16.06 0.074 0.079 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3826 3811 110 34.6 348237.92 22.63 0.047 0.062 0.029 inf-0.60 3641 3628 99 36.6 360491.69 23.09 0.047 0.061 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 965 27 27 100.0 35.7 629845.86 211.94 0.044 0.005 1.01-0.78 1171 28 28 100.0 41.8 318795.45 151.57 0.039 0.005 0.76-0.65 1009 28 28 100.0 36.0 240295.03 123.08 0.055 0.007 0.65-0.59 666 27 27 100.0 24.7 155504.94 91.75 0.074 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3811 110 110 100.0 34.6 348237.92 148.86 0.047 0.006 inf-0.60 3628 99 99 100.0 36.6 360491.69 152.86 0.047 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:18:21 2018) ID: 2932; threads 39; handles 876; mem 518392.00 (1237720.00)kB; time: 1w 5d 1h 23m 51s MEMORY INFO: Memory PF:0.0, Ph:231.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.2,peak PF: 697.1, WS: 296.5, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:231.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.0,peak PF: 697.1, WS: 298.3, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:18:21 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00059 ) 8.37691 ( 0.00062 ) 8.37554 ( 0.00049 ) 90.02113 ( 0.00540 ) 90.03240 ( 0.00528 ) 90.03043 ( 0.00589 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:18:21 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007195 -0.000001 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007175 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000003 0.007185 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(5) 90.021(5) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.36793(19) 8.36793(19) 8.36793(19) 90.0 90.0 90.0 V = 585.94(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb PROFFITPEAK info: 492 peaks in the peak location table UB fit with 240 obs out of 259 (total:259,skipped:0) (92.66%) UB - matrix: -0.025107 -0.079460 -0.015614 ( 0.000047 0.000037 0.000031 ) 0.072243 -0.029492 0.032966 ( 0.000061 0.000047 0.000040 ) -0.036204 -0.003522 0.076481 ( 0.000060 0.000047 0.000040 ) M - matrix: 0.007160 -0.000008 0.000005 ( 0.000010 0.000006 0.000006 ) -0.000008 0.007196 -0.000001 ( 0.000006 0.000006 0.000005 ) 0.000005 -0.000001 0.007180 ( 0.000006 0.000005 0.000007 ) unit cell: 8.382(5) 8.361(4) 8.371(5) 89.99(4) 90.04(5) 89.94(4) V = 586.7(6) UB fit with 240 obs out of 259 (total:259,skipped:0) (92.66%) UB - matrix: -0.025107 -0.079460 -0.015614 ( 0.000047 0.000037 0.000031 ) 0.072243 -0.029492 0.032966 ( 0.000061 0.000047 0.000040 ) -0.036204 -0.003522 0.076481 ( 0.000060 0.000047 0.000040 ) M - matrix: 0.007160 -0.000008 0.000005 ( 0.000010 0.000006 0.000006 ) -0.000008 0.007196 -0.000001 ( 0.000006 0.000006 0.000005 ) 0.000005 -0.000001 0.007180 ( 0.000006 0.000005 0.000007 ) unit cell: 8.382(5) 8.361(4) 8.371(5) 89.99(4) 90.04(5) 89.94(4) V = 586.7(6) OTKP changes: 50 1 1 1 No constraint UB - matrix: -0.025188 -0.079238 -0.015578 ( 0.000046 0.000036 0.000031 ) 0.072095 -0.029576 0.032808 ( 0.000060 0.000047 0.000040 ) -0.036061 -0.003517 0.076307 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007133 -0.000010 0.000006 ( 0.000010 0.000006 0.000006 ) -0.000010 0.007166 -0.000004 ( 0.000006 0.000006 0.000005 ) 0.000006 -0.000004 0.007142 ( 0.000006 0.000005 0.000007 ) Constraint UB - matrix: -0.025188 -0.079238 -0.015578 ( 0.000046 0.000036 0.000031 ) 0.072095 -0.029576 0.032808 ( 0.000060 0.000047 0.000040 ) -0.036061 -0.003517 0.076307 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007142 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007142 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007142 ( 0.000000 0.000000 0.000001 ) UB fit with 242 obs out of 259 (total:259,skipped:0) (93.44%) unit cell: 8.399(5) 8.379(4) 8.393(4) 89.97(4) 90.05(5) 89.92(4) V = 590.7(6) unit cell: 8.3903(8) 8.3903(8) 8.3903(8) 90.0 90.0 90.0 V = 590.66(9) UB fit with 242 obs out of 259 (total:259,skipped:0) (93.44%) UB - matrix: -0.025188 -0.079238 -0.015578 ( 0.000046 0.000036 0.000031 ) 0.072095 -0.029576 0.032808 ( 0.000060 0.000047 0.000040 ) -0.036061 -0.003517 0.076307 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007133 -0.000010 0.000006 ( 0.000010 0.000006 0.000006 ) -0.000010 0.007166 -0.000004 ( 0.000006 0.000006 0.000005 ) 0.000006 -0.000004 0.007142 ( 0.000006 0.000005 0.000007 ) unit cell: 8.399(5) 8.379(4) 8.393(4) 89.97(4) 90.05(5) 89.92(4) V = 590.7(6) OTKP changes: 49 1 1 1 No constraint UB - matrix: -0.025193 -0.079190 -0.015572 ( 0.000046 0.000036 0.000031 ) 0.072068 -0.029570 0.032771 ( 0.000060 0.000047 0.000040 ) -0.036022 -0.003518 0.076287 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007126 -0.000009 0.000006 ( 0.000010 0.000006 0.000006 ) -0.000009 0.007158 -0.000004 ( 0.000006 0.000006 0.000005 ) 0.000006 -0.000004 0.007136 ( 0.000006 0.000005 0.000007 ) Constraint UB - matrix: -0.025193 -0.079190 -0.015572 ( 0.000046 0.000036 0.000031 ) 0.072068 -0.029570 0.032771 ( 0.000060 0.000047 0.000040 ) -0.036022 -0.003518 0.076287 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007136 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007136 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007136 ( 0.000000 0.000000 0.000001 ) UB fit with 242 obs out of 259 (total:259,skipped:0) (93.44%) unit cell: 8.402(5) 8.384(4) 8.397(4) 89.97(4) 90.05(5) 89.93(4) V = 591.5(6) unit cell: 8.3942(8) 8.3942(8) 8.3942(8) 90.0 90.0 90.0 V = 591.49(9) 259 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Run 7 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=53.072) HKL list info: 424 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025193 -0.079190 -0.015572 ( 0.000046 0.000036 0.000031 ) 0.072068 -0.029570 0.032771 ( 0.000060 0.000047 0.000040 ) -0.036022 -0.003518 0.076287 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007126 -0.000009 0.000006 ( 0.000010 0.000006 0.000006 ) -0.000009 0.007158 -0.000004 ( 0.000006 0.000006 0.000005 ) 0.000006 -0.000004 0.007136 ( 0.000006 0.000005 0.000007 ) Constraint UB - matrix: -0.025193 -0.079190 -0.015572 ( 0.000046 0.000036 0.000031 ) 0.072068 -0.029570 0.032771 ( 0.000060 0.000047 0.000040 ) -0.036022 -0.003518 0.076287 ( 0.000059 0.000046 0.000039 ) M - matrix: 0.007136 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007136 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007136 ( 0.000000 0.000000 0.000001 ) UB fit with 242 obs out of 259 (total:259,skipped:0) (93.44%) unit cell: 8.402(5) 8.384(4) 8.397(4) 89.97(4) 90.05(5) 89.93(4) V = 591.5(6) unit cell: 8.3942(8) 8.3942(8) 8.3942(8) 90.0 90.0 90.0 V = 591.49(9) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 243 obs out of 259 (total:259,skipped:0) (93.82%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb 4 of 211 peaks identified as outliers and rejected 207 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 207 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 207 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.10- 1.47 | 21 | 1.030 ( 0.102) | 1.288 ( 0.539) | 1.371 ( 0.825) | 1.42- 1.17 | 21 | 1.004 ( 0.103) | 1.094 ( 0.325) | 1.032 ( 0.467) | 1.17- 0.98 | 21 | 1.010 ( 0.094) | 1.030 ( 0.109) | 0.899 ( 0.348) | 0.97- 0.88 | 21 | 1.017 ( 0.086) | 0.997 ( 0.092) | 1.041 ( 0.368) | 0.88- 0.81 | 21 | 1.015 ( 0.087) | 0.989 ( 0.104) | 1.233 ( 0.549) | 0.81- 0.73 | 21 | 1.003 ( 0.085) | 0.934 ( 0.097) | 1.052 ( 0.343) | 0.73- 0.70 | 21 | 0.964 ( 0.050) | 0.867 ( 0.058) | 1.340 ( 0.674) | 0.70- 0.67 | 21 | 0.947 ( 0.048) | 0.838 ( 0.032) | 1.265 ( 0.551) | 0.66- 0.63 | 21 | 0.943 ( 0.053) | 0.809 ( 0.051) | 1.156 ( 0.438) | 0.62- 0.59 | 18 | 0.902 ( 0.035) | 0.752 ( 0.024) | 1.058 ( 0.401) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.10- 0.59 | 207 | 0.984 ( 0.088) | 0.963 ( 0.259) | 1.146 ( 0.540) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 206 obs out of 207 (total:207,skipped:0) (99.52%) UB - matrix: -0.025222 -0.079176 -0.015651 ( 0.000028 0.000021 0.000019 ) 0.072209 -0.029505 0.032809 ( 0.000035 0.000026 0.000024 ) -0.036043 -0.003374 0.076420 ( 0.000036 0.000027 0.000025 ) M - matrix: 0.007149 -0.000012 0.000009 ( 0.000006 0.000003 0.000004 ) -0.000012 0.007151 0.000013 ( 0.000003 0.000004 0.000003 ) 0.000009 0.000013 0.007161 ( 0.000004 0.000003 0.000004 ) unit cell: 8.389(3) 8.388(2) 8.382(3) 90.11(2) 90.08(3) 89.90(2) V = 589.8(3) OTKP changes: 207 1 1 1 No constraint UB - matrix: -0.025201 -0.079327 -0.015722 ( 0.000027 0.000020 0.000018 ) 0.072307 -0.029541 0.032813 ( 0.000034 0.000025 0.000023 ) -0.036174 -0.003594 0.076541 ( 0.000033 0.000025 0.000023 ) M - matrix: 0.007172 -0.000007 -0.000000 ( 0.000006 0.000003 0.000003 ) -0.000007 0.007178 0.000003 ( 0.000003 0.000004 0.000003 ) -0.000000 0.000003 0.007182 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.025201 -0.079327 -0.015722 ( 0.000027 0.000020 0.000018 ) 0.072307 -0.029541 0.032813 ( 0.000034 0.000025 0.000023 ) -0.036174 -0.003594 0.076541 ( 0.000033 0.000025 0.000023 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000001 ) UB fit with 207 obs out of 207 (total:207,skipped:0) (100.00%) unit cell: 8.375(3) 8.372(2) 8.369(3) 90.02(2) 90.00(3) 89.94(2) V = 586.8(3) unit cell: 8.3722(4) 8.3722(4) 8.3722(4) 90.0 90.0 90.0 V = 586.85(5) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.872) HKL list info: 423 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025201 -0.079327 -0.015722 ( 0.000027 0.000020 0.000018 ) 0.072307 -0.029541 0.032813 ( 0.000034 0.000025 0.000023 ) -0.036174 -0.003594 0.076541 ( 0.000033 0.000025 0.000023 ) M - matrix: 0.007172 -0.000007 -0.000000 ( 0.000006 0.000003 0.000003 ) -0.000007 0.007178 0.000003 ( 0.000003 0.000004 0.000003 ) -0.000000 0.000003 0.007182 ( 0.000003 0.000003 0.000004 ) Constraint UB - matrix: -0.025201 -0.079327 -0.015722 ( 0.000027 0.000020 0.000018 ) 0.072307 -0.029541 0.032813 ( 0.000034 0.000025 0.000023 ) -0.036174 -0.003594 0.076541 ( 0.000033 0.000025 0.000023 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000001 ) UB fit with 207 obs out of 207 (total:207,skipped:0) (100.00%) unit cell: 8.375(3) 8.372(2) 8.369(3) 90.02(2) 90.00(3) 89.94(2) V = 586.8(3) unit cell: 8.3722(4) 8.3722(4) 8.3722(4) 90.0 90.0 90.0 V = 586.85(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 207 obs out of 207 (total:207,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb 2 of 210 peaks identified as outliers and rejected 208 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 208 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 208 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 1.48 | 21 | 1.057 ( 0.165) | 1.369 ( 0.618) | 1.406 ( 0.855) | 1.41- 1.17 | 21 | 1.008 ( 0.103) | 1.112 ( 0.278) | 1.104 ( 0.542) | 1.17- 0.98 | 21 | 1.015 ( 0.094) | 1.029 ( 0.111) | 0.938 ( 0.331) | 0.98- 0.88 | 21 | 1.024 ( 0.080) | 1.016 ( 0.091) | 0.999 ( 0.355) | 0.88- 0.82 | 21 | 1.011 ( 0.096) | 0.997 ( 0.109) | 1.183 ( 0.521) | 0.81- 0.74 | 21 | 1.004 ( 0.088) | 0.937 ( 0.100) | 1.114 ( 0.422) | 0.73- 0.71 | 21 | 0.968 ( 0.052) | 0.877 ( 0.059) | 1.348 ( 0.680) | 0.71- 0.67 | 21 | 0.954 ( 0.049) | 0.853 ( 0.043) | 1.274 ( 0.553) | 0.67- 0.62 | 21 | 0.955 ( 0.043) | 0.817 ( 0.045) | 1.164 ( 0.430) | 0.62- 0.59 | 19 | 0.896 ( 0.040) | 0.754 ( 0.023) | 1.047 ( 0.384) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.05- 0.59 | 208 | 0.990 ( 0.099) | 0.978 ( 0.281) | 1.159 ( 0.550) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 293 | 1.115 ( 0.124) | 1.240 ( 0.474) | 1.253 ( 1.059) | 13.0-18.5 | 293 | 1.074 ( 0.051) | 1.118 ( 0.217) | 1.174 ( 0.509) | 18.6-22.7 | 293 | 1.063 ( 0.074) | 1.133 ( 0.372) | 1.164 ( 0.540) | 22.8-27.1 | 293 | 1.033 ( 0.087) | 1.081 ( 0.282) | 1.145 ( 0.565) | 27.1-30.6 | 293 | 1.006 ( 0.073) | 1.009 ( 0.256) | 1.207 ( 0.495) | 30.6-33.7 | 293 | 0.974 ( 0.074) | 0.925 ( 0.092) | 1.174 ( 0.510) | 33.7-36.9 | 293 | 0.955 ( 0.070) | 0.903 ( 0.113) | 1.149 ( 0.470) | 36.9-39.7 | 293 | 0.935 ( 0.080) | 0.872 ( 0.143) | 1.218 ( 0.562) | 39.7-42.7 | 293 | 0.920 ( 0.071) | 0.837 ( 0.088) | 1.193 ( 0.532) | 42.7-50.1 | 295 | 0.919 ( 0.083) | 0.809 ( 0.065) | 1.148 ( 0.480) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.1 | 2932 | 0.999 ( 0.104) | 0.993 ( 0.283) | 1.182 ( 0.596) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0017 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:18:58 2018 PROFFITMAIN - Started at Tue Mar 27 16:18:58 2018 OTKP changes: 2922 2 4 6 OTKP changes: 2922 2 4 6 No constraint UB - matrix: -0.025048 -0.079524 -0.015610 ( 0.000005 0.000006 0.000006 ) 0.072510 -0.029262 0.032934 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003592 0.076571 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007198 0.000000 0.000005 ( 0.000001 0.000001 0.000001 ) 0.000000 0.007193 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000003 0.007192 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025048 -0.079524 -0.015610 ( 0.000005 0.000006 0.000006 ) 0.072510 -0.029262 0.032934 ( 0.000005 0.000006 0.000006 ) -0.036232 -0.003592 0.076571 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 2927 obs out of 2932 (total:2932,skipped:0) (99.83%) unit cell: 8.3605(5) 8.3631(5) 8.3641(4) 90.021(5) 90.038(5) 90.002(5) V = 584.82(6) unit cell: 8.36257(14) 8.36257(14) 8.36257(14) 90.0 90.0 90.0 V = 584.816(17) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024648 -0.079498 -0.015420 ( 0.000013 0.000011 0.000013 ) 0.072536 -0.028808 0.033014 ( 0.000012 0.000010 0.000011 ) -0.036113 -0.003519 0.076550 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007173 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007188 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3748(11) 8.3812(11) 8.3664(11) 90.043(11) 90.083(11) 89.975(11) V = 587.25(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 808 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007174 -0.000003 0.000009 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007161 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000009 0.000006 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024639 -0.079496 -0.015424 ( 0.000013 0.000011 0.000013 ) 0.072538 -0.028795 0.033011 ( 0.000012 0.000010 0.000011 ) -0.036121 -0.003523 0.076553 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3745(11) 8.3818(11) 8.3662(11) 90.047(11) 90.075(11) 89.978(11) V = 587.25(14) unit cell: 8.3742(4) 8.3742(4) 8.3742(4) 90.0 90.0 90.0 V = 587.25(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024866 -0.079569 -0.015654 ( 0.000013 0.000015 0.000011 ) 0.072445 -0.029195 0.032949 ( 0.000016 0.000018 0.000013 ) -0.036288 -0.003654 0.076368 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000005 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007197 0.000005 ( 0.000002 0.000003 0.000001 ) 0.000005 0.000005 0.007163 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3689(15) 8.3610(15) 8.3809(10) 90.036(12) 90.040(12) 89.969(14) V = 586.42(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024984 -0.079535 -0.015505 ( 0.000017 0.000014 0.000012 ) 0.072504 -0.029256 0.033011 ( 0.000012 0.000010 0.000008 ) -0.036256 -0.003628 0.076513 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007196 -0.000003 0.000007 ( 0.000002 0.000002 0.000001 ) -0.000003 0.007195 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000007 -0.000010 0.007184 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3618(11) 8.3622(14) 8.3683(11) 89.919(12) 90.054(11) 89.980(12) V = 585.13(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007209 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007206 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007197 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3537(11) 8.3555(14) 8.3608(11) 89.935(12) 90.003(11) 89.962(12) V = 583.58(15) unit cell: 8.3567(3) 8.3567(3) 8.3567(3) 90.0 90.0 90.0 V = 583.58(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.740) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007209 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007206 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007197 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3537(11) 8.3555(14) 8.3608(11) 89.935(12) 90.003(11) 89.962(12) V = 583.58(15) unit cell: 8.3567(3) 8.3567(3) 8.3567(3) 90.0 90.0 90.0 V = 583.58(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007209 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007206 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007197 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025027 -0.079595 -0.015467 ( 0.000016 0.000014 0.000012 ) 0.072564 -0.029298 0.032991 ( 0.000011 0.000010 0.000008 ) -0.036296 -0.003559 0.076613 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3537(11) 8.3555(14) 8.3608(11) 89.935(12) 90.003(11) 89.962(12) V = 583.58(15) unit cell: 8.3567(3) 8.3567(3) 8.3567(3) 90.0 90.0 90.0 V = 583.58(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025014 -0.079540 -0.015719 ( 0.000008 0.000013 0.000012 ) 0.072420 -0.029339 0.032917 ( 0.000009 0.000014 0.000014 ) -0.036192 -0.003657 0.076524 ( 0.000008 0.000013 0.000012 ) M - matrix: 0.007180 -0.000003 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007201 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007187 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3707(11) 8.3587(12) 8.3670(11) 90.037(11) 90.060(11) 89.978(11) V = 585.43(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007209 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007203 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3641(10) 8.3538(12) 8.3572(11) 89.996(11) 90.023(10) 90.026(11) V = 583.93(13) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.93(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.740) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007209 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007203 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3641(10) 8.3538(12) 8.3572(11) 89.996(11) 90.023(10) 90.026(11) V = 583.93(13) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.93(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007192 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007209 -0.000000 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000000 0.007203 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025083 -0.079579 -0.015734 ( 0.000008 0.000013 0.000013 ) 0.072412 -0.029374 0.033003 ( 0.000008 0.000014 0.000013 ) -0.036316 -0.003697 0.076594 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3641(10) 8.3538(12) 8.3572(11) 89.996(11) 90.023(10) 90.026(11) V = 583.93(13) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.93(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025237 -0.079454 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072355 -0.029414 0.032793 ( 0.000008 0.000011 0.000012 ) -0.036268 -0.003617 0.076599 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000011 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000011 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3664(10) 8.3643(14) 8.3642(11) 90.091(13) 89.941(10) 90.065(12) V = 585.32(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007200 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007208 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3582(10) 8.3590(14) 8.3545(11) 90.051(12) 89.991(10) 90.064(12) V = 583.70(14) unit cell: 8.3572(3) 8.3572(3) 8.3572(3) 90.0 90.0 90.0 V = 583.70(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.740) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007200 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007208 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3582(10) 8.3590(14) 8.3545(11) 90.051(12) 89.991(10) 90.064(12) V = 583.70(14) unit cell: 8.3572(3) 8.3572(3) 8.3572(3) 90.0 90.0 90.0 V = 583.70(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007200 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007208 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025250 -0.079508 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072481 -0.029416 0.032810 ( 0.000008 0.000011 0.000012 ) -0.036203 -0.003661 0.076704 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3582(10) 8.3590(14) 8.3545(11) 90.051(12) 89.991(10) 90.064(12) V = 583.70(14) unit cell: 8.3572(3) 8.3572(3) 8.3572(3) 90.0 90.0 90.0 V = 583.70(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025308 -0.079451 -0.015629 ( 0.000010 0.000008 0.000010 ) 0.072447 -0.029435 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036123 -0.003527 0.076575 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000006 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000006 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007184 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3627(13) 8.3642(9) 8.3687(12) 90.050(10) 90.043(12) 90.046(10) V = 585.37(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007201 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007198 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007206 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3585(13) 8.3605(9) 8.3556(12) 90.066(10) 90.050(12) 90.026(10) V = 583.90(14) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.740) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007201 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007198 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007206 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3585(13) 8.3605(9) 8.3556(12) 90.066(10) 90.050(12) 90.026(10) V = 583.90(14) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007201 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007198 0.000008 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000008 0.007206 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079471 -0.015726 ( 0.000011 0.000008 0.000010 ) 0.072504 -0.029483 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003580 0.076703 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3585(13) 8.3605(9) 8.3556(12) 90.066(10) 90.050(12) 90.026(10) V = 583.90(14) unit cell: 8.3582(3) 8.3582(3) 8.3582(3) 90.0 90.0 90.0 V = 583.90(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 208 obs out of 208 (total:208,skipped:0) (100.00%) UB - matrix: -0.025179 -0.079329 -0.015678 ( 0.000031 0.000023 0.000021 ) 0.072331 -0.029523 0.032911 ( 0.000035 0.000026 0.000024 ) -0.036192 -0.003463 0.076586 ( 0.000038 0.000028 0.000026 ) M - matrix: 0.007176 -0.000013 0.000003 ( 0.000006 0.000003 0.000004 ) -0.000013 0.007177 0.000007 ( 0.000003 0.000004 0.000003 ) 0.000003 0.000007 0.007194 ( 0.000004 0.000003 0.000004 ) unit cell: 8.373(3) 8.373(2) 8.362(3) 90.05(3) 90.03(3) 89.90(3) V = 586.3(3) OTKP changes: 208 1 1 1 No constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007173 -0.000008 -0.000001 ( 0.000006 0.000003 0.000004 ) -0.000008 0.007179 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000001 0.000001 0.007184 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 208 obs out of 208 (total:208,skipped:0) (100.00%) unit cell: 8.375(3) 8.371(2) 8.368(3) 90.01(2) 89.99(3) 89.94(3) V = 586.7(3) unit cell: 8.3716(5) 8.3716(5) 8.3716(5) 90.0 90.0 90.0 V = 586.72(6) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.865) HKL list info: 418 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007173 -0.000008 -0.000001 ( 0.000006 0.000003 0.000004 ) -0.000008 0.007179 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000001 0.000001 0.007184 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 208 obs out of 208 (total:208,skipped:0) (100.00%) unit cell: 8.375(3) 8.371(2) 8.368(3) 90.01(2) 89.99(3) 89.94(3) V = 586.7(3) unit cell: 8.3716(5) 8.3716(5) 8.3716(5) 90.0 90.0 90.0 V = 586.72(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 208 obs out of 208 (total:208,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007173 -0.000008 -0.000001 ( 0.000006 0.000003 0.000004 ) -0.000008 0.007179 0.000001 ( 0.000003 0.000004 0.000003 ) -0.000001 0.000001 0.007184 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025199 -0.079326 -0.015718 ( 0.000032 0.000024 0.000022 ) 0.072305 -0.029554 0.032818 ( 0.000034 0.000025 0.000023 ) -0.036187 -0.003603 0.076552 ( 0.000035 0.000026 0.000024 ) M - matrix: 0.007174 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007174 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007174 ( 0.000000 0.000000 0.000001 ) UB fit with 208 obs out of 208 (total:208,skipped:0) (100.00%) unit cell: 8.375(3) 8.371(2) 8.368(3) 90.01(2) 89.99(3) 89.94(3) V = 586.7(3) unit cell: 8.3716(5) 8.3716(5) 8.3716(5) 90.0 90.0 90.0 V = 586.72(6) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025040 -0.079451 -0.015590 ( 0.000006 0.000006 0.000006 ) 0.072502 -0.029251 0.032885 ( 0.000006 0.000007 0.000007 ) -0.036228 -0.003597 0.076566 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000001 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007181 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.000001 0.007187 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025040 -0.079451 -0.015590 ( 0.000006 0.000006 0.000006 ) 0.072502 -0.029251 0.032885 ( 0.000006 0.000007 0.000007 ) -0.036228 -0.003597 0.076566 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) UB fit with 2927 obs out of 2932 (total:2932,skipped:0) (99.83%) unit cell: 8.3615(6) 8.3702(6) 8.3668(5) 90.010(5) 90.006(5) 89.992(6) V = 585.58(7) unit cell: 8.36619(19) 8.36619(19) 8.36619(19) 90.0 90.0 90.0 V = 585.58(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 73 reflections under beam stop or inside a detector rejection region 23 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof 3978 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:19:07 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.740) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.740) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.740) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.740) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.865) PROFFIT INFO: signal sum: min=101.0000 max=23085540.0000 PROFFIT INFO: signal sum lp corr: min=411.4004 max=3187619.9189 PROFFIT INFO: background sum: min=612.0000 max=26038.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11900.0000 PROFFIT INFO: num of signal pixels: min=51 max=543 PROFFIT INFO: Inet: min=658.2407 max=5100192.0000 PROFFIT INFO: sig(Inet): min=120.2006 max=47805.8867 PROFFIT INFO: Inet/sig(Inet): min=0.70 max=248.37 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 51 206 441 816 924 1682 2678 3658 3978 Percent 0.0 0.1 1.3 5.2 11.1 20.5 23.2 42.3 67.3 92.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3978 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3978 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100192- 1105318 397 1839685.54 121.50 100.00 1095690- 606512 397 824551.07 101.58 100.00 601591- 253958 397 397429.35 93.13 100.00 253774- 164858 397 197140.53 70.55 100.00 164810- 115951 397 139440.99 49.82 100.00 115682- 87827 397 100999.93 35.07 100.00 87778- 61924 397 75863.03 28.26 100.00 61796- 5285 397 33662.99 18.31 100.00 5284- 2846 397 3755.55 5.21 95.97 2841- 658 405 2021.67 3.64 53.09 ------------------------------------------------------------------------------------ 5100192- 658 3978 360732.22 52.61 94.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 750707.85 91.51 100.00 1.41- 1.12 397 582365.31 63.92 99.24 1.12- 0.96 397 503966.44 70.42 97.48 0.96- 0.88 397 336427.97 58.52 93.70 0.88- 0.81 397 438244.68 67.86 99.50 0.81- 0.73 397 238821.67 40.57 95.47 0.73- 0.71 397 170990.21 33.97 88.66 0.71- 0.65 397 301054.87 46.39 93.45 0.65- 0.62 397 146634.81 26.67 86.90 0.62- 0.58 405 142505.94 26.74 93.83 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 360732.22 52.61 94.82 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:19:07 2018 Sorting 3978 observations 119 unique observations with > 7.00 F2/sig(F2) 3978 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 48 677 Total number of frames 677 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 3978 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 8 116 Total number of frames 116 3186 observations > 7.00 F2/sig(F2) 3186 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 8 116 Total number of frames 116 Removing 'redundancy=1' reflections Average redundancy: 24.5 (Out of 3186 removed 3 = 3183, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3183 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 8 116 Total number of frames 116 130 unique data precomputed (should be 130) 130 unique data with 3183 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 24.5 (Out of 3183 removed 0 = 3183, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3183 observations RMS deviation of equivalent data = 0.26734 Rint = 0.20052 8 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19441, wR= 0.28145 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15504, wR= 0.20491, Acormin=0.578, Acormax=1.344, Acor_av=0.992 F test: Probability=1.000, F= 1.570 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13177, wR= 0.16760, Acormin=0.504, Acormax=1.431, Acor_av=0.908 F test: Probability=1.000, F= 1.383 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13076, wR= 0.17638, Acormin=0.580, Acormax=1.603, Acor_av=0.975 F test: Probability=0.644, F= 1.013 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10252, wR= 0.13852, Acormin=0.451, Acormax=1.559, Acor_av=0.899 F test: Probability=1.000, F= 1.647 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09142, wR= 0.12528, Acormin=0.447, Acormax=1.607, Acor_av=0.915 F test: Probability=1.000, F= 1.255 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11616, wR= 0.16138, Acormin=0.622, Acormax=1.664, Acor_av=0.984 F test: Probability=0.000, F= 0.619 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09270, wR= 0.12908, Acormin=0.467, Acormax=1.663, Acor_av=0.911 F test: Probability=0.000, F= 0.971 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08445, wR= 0.11834, Acormin=0.458, Acormax=1.652, Acor_av=0.923 F test: Probability=1.000, F= 1.167 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08078, wR= 0.11141, Acormin=0.329, Acormax=1.531, Acor_av=0.871 F test: Probability=0.990, F= 1.089 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11973, wR= 0.15717, Acormin=0.414, Acormax=1.436, Acor_av=0.812 F test: Probability=0.000, F= 0.456 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09170, wR= 0.12550, Acormin=0.447, Acormax=1.624, Acor_av=0.897 F test: Probability=0.000, F= 0.776 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09366, wR= 0.12389, Acormin=0.077, Acormax=0.339, Acor_av=0.181 F test: Probability=0.000, F= 0.742 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08476, wR= 0.11369, Acormin=0.075, Acormax=0.375, Acor_av=0.201 F test: Probability=0.000, F= 0.903 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07748, wR= 0.10458, Acormin=0.078, Acormax=0.402, Acor_av=0.212 F test: Probability=0.977, F= 1.076 Final absorption model (ne=6, no=5): Rint= 0.08078, Acormin=0.329, Acormax=1.531, Acor_av=0.871 Combined refinement in use Rint: 0.20063 There are 116 active scales (one needs to be fixed) Refinement control: frame scale #110 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 163 pars with 13366 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26734 Using Levenberg-Marquardt: 0.00010 New wR= 0.06742 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20052 with corrections 0.05235 Rint for all data: 0.20063 with corrections 0.05257 0 observations identified as outliers and rejected Cycle 2 wR= 0.06742 Using Levenberg-Marquardt: 0.00001 New wR= 0.06297 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20052 with corrections 0.04875 Rint for all data: 0.20063 with corrections 0.04898 0 observations identified as outliers and rejected Cycle 3 wR= 0.06297 Using Levenberg-Marquardt: 0.00000 New wR= 0.06186 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20052 with corrections 0.04800 Rint for all data: 0.20063 with corrections 0.04823 0 observations identified as outliers and rejected Cycle 4 wR= 0.06186 Using Levenberg-Marquardt: 0.00000 New wR= 0.06126 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20052 with corrections 0.04762 Rint for all data: 0.20063 with corrections 0.04785 0 observations identified as outliers and rejected Cycle 5 wR= 0.06126 Using Levenberg-Marquardt: 0.00000 New wR= 0.06087 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20052 with corrections 0.04737 Rint for all data: 0.20063 with corrections 0.04760 0 observations identified as outliers and rejected Final wR= 0.06087 Final frame scales: Min= 0.7752 Max= 1.3407 Final absorption correction factors: Amin= 0.4564 Amax= 1.5027 PROFFIT INFO: Inet (after scale3 abspack): min=708.5942 max=4481153.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=136.4706 max=54460.5313 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 3978 reflections read from tmp file 860 reflections are rejected (860 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 4 3 4 4 2 4 3 5 127 Initial Chi^2= 0.41686 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.91681 Current error model SIG(F2)^2 = 140.87*I_RAW + 0.00*I_BACK+(0.01873*)^2 Cycle 2, Chi^2= 1.00300 Current error model SIG(F2)^2 = 106.90*I_RAW + 0.00*I_BACK+(0.02232*)^2 Cycle 3, Chi^2= 1.00021 Current error model SIG(F2)^2 = 111.06*I_RAW + 0.00*I_BACK+(0.02145*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 110.62*I_RAW + 0.00*I_BACK+(0.02156*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 110.68*I_RAW + 0.00*I_BACK+(0.02155*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 110.68*I_RAW + 0.00*I_BACK+(0.02155*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4481154- 1052094 397 1713240.88 43.48 100.00 1049211- 580362 397 779782.39 36.87 100.00 579015- 246346 397 384915.26 35.45 100.00 246173- 147591 397 183317.82 31.23 100.00 147452- 117668 397 132907.58 25.36 100.00 117658- 83282 397 96588.75 19.52 100.00 83279- 64087 397 74163.45 16.79 100.00 64042- 4687 397 36158.20 11.82 100.00 4629- 2662 397 3463.12 4.68 96.73 2662- 709 405 2041.79 3.79 74.07 ------------------------------------------------------------------------------------ 4481154- 709 3978 339976.95 22.86 97.03 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 745723.21 35.47 100.00 1.41- 1.12 397 556563.63 28.08 99.50 1.12- 0.96 397 456882.17 27.39 97.98 0.96- 0.88 397 311606.34 23.47 96.98 0.88- 0.81 397 409521.42 27.00 99.75 0.81- 0.73 397 216686.90 18.71 97.48 0.73- 0.71 397 161815.36 17.49 91.94 0.71- 0.65 397 279273.05 22.00 97.73 0.65- 0.62 397 136109.26 14.41 92.44 0.62- 0.58 405 129822.98 14.76 96.54 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 339976.95 22.86 97.03 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 745723.21 35.47 100.00 4.82- 1.12 794 651143.42 31.78 99.75 4.82- 0.96 1191 586389.67 30.31 99.16 4.82- 0.88 1588 517693.83 28.60 98.61 4.82- 0.81 1985 496059.35 28.28 98.84 4.82- 0.73 2382 449497.28 26.69 98.61 4.82- 0.71 2779 408399.86 25.37 97.66 4.82- 0.65 3176 392259.01 24.95 97.67 4.82- 0.62 3573 363797.92 23.78 97.09 4.82- 0.58 3978 339976.95 22.86 97.03 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 339976.95 22.86 97.03 Scale applied to data: s=0.223157 (maximum obs:4481153.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.028: data 3978 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.028: data 3964 -> merged 157 Rejected total: 14, method kkm 10, method Blessing 4 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585750, 4.830220 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.48 14 14 23.36 100.00 327 1.41 - 1.12 14 14 32.57 100.00 456 1.12 - 0.97 14 14 32.64 100.00 457 0.96 - 0.84 14 14 34.64 100.00 485 0.84 - 0.78 14 14 26.57 100.00 372 0.78 - 0.73 14 14 27.86 100.00 390 0.73 - 0.69 14 14 26.07 100.00 365 0.69 - 0.66 14 14 22.29 100.00 312 0.65 - 0.63 14 14 23.21 100.00 325 0.63 - 0.60 14 14 20.50 100.00 287 --------------------------------------------------------------- 8.38 - 0.60 140 140 26.97 100.00 3776 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:19:08 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361516 8.370242 8.366805 90.0104 90.0058 89.9922 3964 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2020 0 2658 2656 3964 N (int>3sigma) = 0 0 0 0 2020 0 2579 2573 3846 Mean intensity = 0.0 0.0 0.0 0.0 29.9 0.0 76.4 78.0 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 22.9 23.0 22.9 Lattice type: F chosen Volume: 585.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.914 5.915 5.915 119.97 119.97 90.04 Niggli form: a.a = 34.976 b.b = 34.983 c.c = 34.989 b.c = -17.475 a.c = -17.478 a.b = -0.022 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.046 CUBIC F-lattice R(int) = 0.047 [ 3807] Vol = 585.6 Cell: 8.370 8.367 8.362 89.99 90.01 90.01 Volume: 585.58 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.015 TETRAGONAL I-lattice R(int) = 0.046 [ 3557] Vol = 292.8 Cell: 5.918 5.917 8.362 90.00 89.99 89.98 Volume: 292.79 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.029 TETRAGONAL I-lattice R(int) = 0.046 [ 3551] Vol = 292.8 Cell: 5.914 5.915 8.370 89.99 90.00 90.04 Volume: 292.79 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.021 TETRAGONAL I-lattice R(int) = 0.046 [ 3557] Vol = 292.8 Cell: 5.917 5.918 8.362 90.01 90.00 90.02 Volume: 292.79 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.046 [ 3515] Vol = 585.6 Cell: 8.362 8.367 8.370 90.01 90.01 89.99 Volume: 585.58 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3503] Vol = 292.8 Cell: 8.362 5.917 5.918 89.98 89.99 90.00 Volume: 292.79 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.030 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3499] Vol = 292.8 Cell: 5.914 5.915 8.370 90.01 90.00 90.04 Volume: 292.79 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.008 MONOCLINIC I-lattice R(int) = 0.043 [ 3168] Vol = 292.8 Cell: 5.917 8.362 5.918 90.01 90.02 90.00 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.009 MONOCLINIC I-lattice R(int) = 0.044 [ 3164] Vol = 292.8 Cell: 5.915 8.367 5.916 89.99 90.06 90.00 Volume: 292.79 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.008 MONOCLINIC I-lattice R(int) = 0.043 [ 3168] Vol = 292.8 Cell: 5.917 8.362 5.918 90.01 90.02 90.00 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.024 MONOCLINIC I-lattice R(int) = 0.044 [ 3149] Vol = 292.8 Cell: 5.915 5.914 8.370 90.00 90.01 89.96 Volume: 292.79 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.006 MONOCLINIC I-lattice R(int) = 0.045 [ 3162] Vol = 292.8 Cell: 5.914 8.370 5.915 89.99 90.04 90.00 Volume: 292.79 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.011 MONOCLINIC I-lattice R(int) = 0.045 [ 3162] Vol = 292.8 Cell: 5.914 8.370 5.915 90.01 90.04 90.00 Volume: 292.79 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2474] Vol = 146.4 Cell: 5.914 5.915 5.915 119.97 119.97 90.04 Volume: 146.39 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2020 0 2655 2656 3964 N (int>3sigma) = 0 0 0 0 2020 0 2569 2573 3846 Mean intensity = 0.0 0.0 0.0 0.0 29.9 0.0 75.4 78.0 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 22.9 23.0 22.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 299 883 N I>3s 42 42 286 883 0.9 0.9 0.7 35.4 9.3 9.3 5.5 26.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3528 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3567 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370242 8.366805 8.361516 89.9942 90.0078 90.0104 ZERR 3.00 0.000609 0.000488 0.000607 0.0054 0.0059 0.0053 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3795088- 715624 650 649 26 25.0 1378263.06 41.31 0.042 0.056 705487- 215436 611 608 26 23.4 430075.63 35.55 0.060 0.075 210277- 92908 919 919 26 35.3 141574.68 26.07 0.045 0.059 89871- 63935 650 648 26 24.9 77937.21 17.02 0.069 0.088 61212- 3401 507 503 26 19.3 23537.76 8.98 0.087 0.118 3277- 1651 641 637 27 23.6 2537.09 4.28 0.198 0.257 ------------------------------------------------------------------------------------------- 3795088- 1651 3978 3964 157 25.2 340576.38 22.87 0.047 0.062 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 746 740 26 28.5 600636.39 31.10 0.046 0.062 0.023 1.12-0.88 876 874 26 33.6 437652.26 26.56 0.035 0.047 0.026 0.85-0.75 736 736 26 28.3 312200.15 22.38 0.045 0.056 0.030 0.74-0.68 644 643 26 24.7 248740.47 20.27 0.060 0.071 0.033 0.67-0.63 613 612 26 23.5 138243.24 15.85 0.073 0.090 0.042 0.62-0.59 363 359 27 13.3 135770.11 14.54 0.075 0.077 0.043 ------------------------------------------------------------------------------------------------------ inf-0.59 3978 3964 157 25.2 340576.38 22.87 0.047 0.062 0.028 inf-0.60 3785 3774 139 27.2 352747.08 23.34 0.047 0.062 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 740 26 26 100.0 28.5 600636.39 179.31 0.046 0.005 1.12-0.88 874 26 26 100.0 33.6 437652.26 156.98 0.035 0.005 0.85-0.75 736 26 26 100.0 28.3 312200.15 126.23 0.045 0.006 0.74-0.68 643 26 26 100.0 24.7 248740.47 103.35 0.060 0.007 0.67-0.63 612 26 26 100.0 23.5 138243.24 76.21 0.073 0.009 0.62-0.59 359 27 27 100.0 13.3 135770.11 60.36 0.075 0.016 -------------------------------------------------------------------------------------------- inf-0.59 3964 157 157 100.0 25.2 340576.38 125.52 0.047 0.007 inf-0.60 3774 139 139 100.0 27.2 352747.08 129.33 0.047 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025040 -0.079450 -0.015590 ( 0.000006 0.000006 0.000006 ) 0.072502 -0.029250 0.032885 ( 0.000006 0.000007 0.000007 ) -0.036228 -0.003597 0.076567 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000001 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007181 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.000001 0.007187 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025040 -0.079450 -0.015590 ( 0.000006 0.000006 0.000006 ) 0.072502 -0.029250 0.032885 ( 0.000006 0.000007 0.000007 ) -0.036228 -0.003597 0.076567 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007187 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007187 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007187 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3615(6) 8.3703(6) 8.3668(5) 90.010(5) 90.006(5) 89.992(6) V = 585.58(7) unit cell: 8.36620(19) 8.36620(19) 8.36620(19) 90.0 90.0 90.0 V = 585.58(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.740) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.740) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.740) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.740) Run 7 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.865) PROFFIT INFO: signal sum: min=101.0000 max=23085540.0000 PROFFIT INFO: signal sum lp corr: min=411.4004 max=3187619.9189 PROFFIT INFO: background sum: min=612.0000 max=26038.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=11900.0000 PROFFIT INFO: num of signal pixels: min=51 max=543 PROFFIT INFO: Inet: min=658.2407 max=5100192.0000 PROFFIT INFO: sig(Inet): min=120.2006 max=47805.8867 PROFFIT INFO: Inet/sig(Inet): min=0.70 max=248.37 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 102 412 882 1632 1848 3364 5356 7316 7956 Percent 0.0 0.1 1.3 5.2 11.1 20.5 23.2 42.3 67.3 92.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 3978 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 3978 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100192- 1105318 397 1839685.54 121.50 100.00 1095690- 606512 397 824551.07 101.58 100.00 601591- 253958 397 397429.35 93.13 100.00 253774- 164858 397 197140.53 70.55 100.00 164810- 115951 397 139440.99 49.82 100.00 115682- 87827 397 100999.93 35.07 100.00 87778- 61924 397 75863.03 28.26 100.00 61796- 5285 397 33662.99 18.31 100.00 5284- 2846 397 3755.55 5.21 95.97 2841- 658 405 2021.67 3.64 53.09 ------------------------------------------------------------------------------------ 5100192- 658 3978 360732.22 52.61 94.82 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 750707.85 91.51 100.00 1.41- 1.12 397 582365.31 63.92 99.24 1.12- 0.96 397 503966.44 70.42 97.48 0.96- 0.88 397 336427.97 58.52 93.70 0.88- 0.81 397 438244.68 67.86 99.50 0.81- 0.73 397 238821.67 40.57 95.47 0.73- 0.71 397 170990.21 33.97 88.66 0.71- 0.65 397 301054.87 46.39 93.45 0.65- 0.62 397 146634.81 26.67 86.90 0.62- 0.58 405 142505.94 26.74 93.83 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 360732.22 52.61 94.82 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:19:09 2018 Sorting 3978 observations 86 unique observations with > 7.00 F2/sig(F2) 3978 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 48 677 Total number of frames 677 Maximum number of 86 frame scales suggested for reliable scaling Glued frame scales: 8 frame = 1 scale 3978 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 6 89 Total number of frames 89 3186 observations > 7.00 F2/sig(F2) 3186 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 6 89 Total number of frames 89 Removing 'redundancy=1' reflections Average redundancy: 34.2 (Out of 3186 removed 3 = 3183, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3183 observations in 7 runs Run # start # end # total # 1 0 13 14 2 0 12 27 3 0 13 41 4 0 13 55 5 0 12 68 6 0 13 82 7 0 6 89 Total number of frames 89 93 unique data precomputed (should be 93) 93 unique data with 3183 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 34.2 (Out of 3183 removed 0 = 3183, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3183 observations RMS deviation of equivalent data = 0.26807 Rint = 0.20080 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19593, wR= 0.28480 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15588, wR= 0.20621, Acormin=0.576, Acormax=1.345, Acor_av=0.992 F test: Probability=1.000, F= 1.577 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13213, wR= 0.16832, Acormin=0.502, Acormax=1.432, Acor_av=0.908 F test: Probability=1.000, F= 1.390 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13125, wR= 0.17725, Acormin=0.581, Acormax=1.603, Acor_av=0.976 F test: Probability=0.623, F= 1.011 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10251, wR= 0.13910, Acormin=0.449, Acormax=1.559, Acor_av=0.900 F test: Probability=1.000, F= 1.657 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09149, wR= 0.12573, Acormin=0.442, Acormax=1.610, Acor_av=0.916 F test: Probability=1.000, F= 1.252 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11600, wR= 0.16194, Acormin=0.623, Acormax=1.666, Acor_av=0.987 F test: Probability=0.000, F= 0.622 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09291, wR= 0.12935, Acormin=0.468, Acormax=1.659, Acor_av=0.914 F test: Probability=0.000, F= 0.968 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08443, wR= 0.11858, Acormin=0.459, Acormax=1.663, Acor_av=0.925 F test: Probability=1.000, F= 1.169 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08119, wR= 0.11216, Acormin=0.329, Acormax=1.536, Acor_av=0.872 F test: Probability=0.980, F= 1.077 Trying model 10 (ne=8, no=0)... Results: Rint= 0.12004, wR= 0.15754, Acormin=0.418, Acormax=1.429, Acor_av=0.814 F test: Probability=0.000, F= 0.458 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09174, wR= 0.12561, Acormin=0.451, Acormax=1.622, Acor_av=0.899 F test: Probability=0.000, F= 0.783 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09417, wR= 0.12468, Acormin=0.076, Acormax=0.335, Acor_av=0.178 F test: Probability=0.000, F= 0.742 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08542, wR= 0.11506, Acormin=0.074, Acormax=0.369, Acor_av=0.197 F test: Probability=0.000, F= 0.898 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07804, wR= 0.10593, Acormin=0.075, Acormax=0.394, Acor_av=0.207 F test: Probability=0.970, F= 1.071 Final absorption model (ne=6, no=5): Rint= 0.08119, Acormin=0.329, Acormax=1.536, Acor_av=0.872 Combined refinement in use Rint: 0.20091 There are 89 active scales (one needs to be fixed) Refinement control: frame scale #9 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 136 pars with 9316 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26807 Using Levenberg-Marquardt: 0.00010 New wR= 0.06925 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.05365 Rint for all data: 0.20091 with corrections 0.05387 0 observations identified as outliers and rejected Cycle 2 wR= 0.06925 Using Levenberg-Marquardt: 0.00001 New wR= 0.06475 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.05000 Rint for all data: 0.20091 with corrections 0.05023 0 observations identified as outliers and rejected Cycle 3 wR= 0.06475 Using Levenberg-Marquardt: 0.00000 New wR= 0.06330 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.04905 Rint for all data: 0.20091 with corrections 0.04928 0 observations identified as outliers and rejected Cycle 4 wR= 0.06330 Using Levenberg-Marquardt: 0.00000 New wR= 0.06240 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.04852 Rint for all data: 0.20091 with corrections 0.04875 0 observations identified as outliers and rejected Cycle 5 wR= 0.06240 Using Levenberg-Marquardt: 0.00000 New wR= 0.06178 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20080 with corrections 0.04817 Rint for all data: 0.20091 with corrections 0.04840 0 observations identified as outliers and rejected Final wR= 0.06178 Final frame scales: Min= 0.7951 Max= 1.2730 Final absorption correction factors: Amin= 0.4623 Amax= 1.4818 PROFFIT INFO: Inet (after scale3 abspack): min=705.3408 max=4473791.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=134.7662 max=52448.1797 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 3978 reflections read from tmp file 868 reflections are rejected (868 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 3 5 0 2 3 2 3 91 Initial Chi^2= 0.41156 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93109 Current error model SIG(F2)^2 = 151.49*I_RAW + 0.00*I_BACK+(0.01771*)^2 Cycle 2, Chi^2= 1.00707 Current error model SIG(F2)^2 = 107.99*I_RAW + 0.00*I_BACK+(0.02270*)^2 Cycle 3, Chi^2= 1.00039 Current error model SIG(F2)^2 = 115.05*I_RAW + 0.00*I_BACK+(0.02142*)^2 Cycle 4, Chi^2= 0.99998 Current error model SIG(F2)^2 = 114.22*I_RAW + 0.00*I_BACK+(0.02160*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 114.36*I_RAW + 0.00*I_BACK+(0.02158*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 114.36*I_RAW + 0.00*I_BACK+(0.02158*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4473792- 1049859 397 1714781.78 43.33 100.00 1049458- 578820 397 780268.11 36.68 100.00 578061- 246589 397 384538.01 35.16 100.00 246356- 147270 397 183826.56 31.01 100.00 147190- 117622 397 133121.34 24.95 100.00 117612- 83159 397 96375.44 19.27 100.00 83140- 64152 397 74210.93 16.61 100.00 64096- 4702 397 36156.90 11.64 99.75 4689- 2656 397 3464.30 4.60 95.72 2654- 705 405 2043.04 3.73 72.10 ------------------------------------------------------------------------------------ 4473792- 705 3978 340197.22 22.66 96.71 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 744981.34 35.30 100.00 1.41- 1.12 397 558045.04 27.91 99.50 1.12- 0.96 397 456946.48 27.17 97.98 0.96- 0.88 397 312562.96 23.25 96.22 0.88- 0.81 397 409748.25 26.76 99.75 0.81- 0.73 397 217076.49 18.51 97.23 0.73- 0.71 397 161869.83 17.29 90.93 0.71- 0.65 397 279157.80 21.77 97.73 0.65- 0.62 397 136125.73 14.23 91.69 0.62- 0.58 405 129700.08 14.57 96.05 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 340197.22 22.66 96.71 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 397 744981.34 35.30 100.00 4.82- 1.12 794 651513.19 31.61 99.75 4.82- 0.96 1191 586657.62 30.13 99.16 4.82- 0.88 1588 518133.95 28.41 98.43 4.82- 0.81 1985 496456.81 28.08 98.69 4.82- 0.73 2382 449893.43 26.48 98.45 4.82- 0.71 2779 408747.20 25.17 97.37 4.82- 0.65 3176 392548.52 24.75 97.42 4.82- 0.62 3573 364057.10 23.58 96.78 4.82- 0.58 3978 340197.22 22.66 96.71 ------------------------------------------------------------------------------------ 4.82- 0.58 3978 340197.22 22.66 96.71 Scale applied to data: s=0.223524 (maximum obs:4473791.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.048; Rsigma 0.029: data 3978 -> merged 110 With outlier rejection... Rint 0.048; Rsigma 0.029: data 3962 -> merged 110 Rejected total: 16, method kkm 11, method Blessing 5 Completeness direct cell (a, b, c) = (8.366, 8.366, 8.366), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585751, 4.830227 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.71 10 10 24.90 100.00 249 1.61 - 1.21 10 10 36.50 100.00 365 1.17 - 1.01 10 10 47.10 100.00 471 0.99 - 0.89 10 10 45.70 100.00 457 0.88 - 0.81 10 10 43.90 100.00 439 0.81 - 0.74 10 10 38.40 100.00 384 0.73 - 0.71 10 10 41.90 100.00 419 0.70 - 0.66 10 10 35.10 100.00 351 0.66 - 0.64 10 10 32.70 100.00 327 0.63 - 0.60 10 10 31.10 100.00 311 --------------------------------------------------------------- 8.38 - 0.60 100 100 37.73 100.00 3773 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:19:08 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.361516 8.370242 8.366805 90.0104 90.0058 89.9922 3964 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.87 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2020 0 2658 2656 3964 N (int>3sigma) = 0 0 0 0 2020 0 2579 2573 3846 Mean intensity = 0.0 0.0 0.0 0.0 29.9 0.0 76.4 78.0 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 22.9 23.0 22.9 Lattice type: F chosen Volume: 585.58 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Unitcell: 5.914 5.915 5.915 119.97 119.97 90.04 Niggli form: a.a = 34.976 b.b = 34.983 c.c = 34.989 b.c = -17.475 a.c = -17.478 a.b = -0.022 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.046 CUBIC F-lattice R(int) = 0.047 [ 3807] Vol = 585.6 Cell: 8.370 8.367 8.362 89.99 90.01 90.01 Volume: 585.58 Matrix: 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.015 TETRAGONAL I-lattice R(int) = 0.046 [ 3557] Vol = 292.8 Cell: 5.918 5.917 8.362 90.00 89.99 89.98 Volume: 292.79 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [15] err= 0.029 TETRAGONAL I-lattice R(int) = 0.046 [ 3551] Vol = 292.8 Cell: 5.914 5.915 8.370 89.99 90.00 90.04 Volume: 292.79 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.021 TETRAGONAL I-lattice R(int) = 0.046 [ 3557] Vol = 292.8 Cell: 5.917 5.918 8.362 90.01 90.00 90.02 Volume: 292.79 Matrix: 0.0000 0.5000 0.5000 0.0000 -0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [16] err= 0.011 ORTHORHOMBIC F-lattice R(int) = 0.046 [ 3515] Vol = 585.6 Cell: 8.362 8.367 8.370 90.01 90.01 89.99 Volume: 585.58 Matrix:-1.0000 0.0000 0.0000 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3503] Vol = 292.8 Cell: 8.362 5.917 5.918 89.98 89.99 90.00 Volume: 292.79 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 ------------------------------------------------------------------------------ Option: [42] err= 0.030 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3499] Vol = 292.8 Cell: 5.914 5.915 8.370 90.01 90.00 90.04 Volume: 292.79 Matrix:-0.5000 0.0000 -0.5000 -0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.008 MONOCLINIC I-lattice R(int) = 0.043 [ 3168] Vol = 292.8 Cell: 5.917 8.362 5.918 90.01 90.02 90.00 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [14] err= 0.009 MONOCLINIC I-lattice R(int) = 0.044 [ 3164] Vol = 292.8 Cell: 5.915 8.367 5.916 89.99 90.06 90.00 Volume: 292.79 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.008 MONOCLINIC I-lattice R(int) = 0.043 [ 3168] Vol = 292.8 Cell: 5.917 8.362 5.918 90.01 90.02 90.00 Volume: 292.79 Matrix: 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 0.0000 0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [37] err= 0.024 MONOCLINIC I-lattice R(int) = 0.044 [ 3149] Vol = 292.8 Cell: 5.915 5.914 8.370 90.00 90.01 89.96 Volume: 292.79 Matrix:-0.5000 0.0000 0.5000 0.5000 0.0000 0.5000 0.0000 1.0000 0.0000 ------------------------------------------------------------------------------ Option: [43] err= 0.006 MONOCLINIC I-lattice R(int) = 0.045 [ 3162] Vol = 292.8 Cell: 5.914 8.370 5.915 89.99 90.04 90.00 Volume: 292.79 Matrix:-0.5000 0.0000 -0.5000 0.0000 -1.0000 0.0000 -0.5000 0.0000 0.5000 ------------------------------------------------------------------------------ Option: [25] err= 0.011 MONOCLINIC I-lattice R(int) = 0.045 [ 3162] Vol = 292.8 Cell: 5.914 8.370 5.915 90.01 90.04 90.00 Volume: 292.79 Matrix: 0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2474] Vol = 146.4 Cell: 5.914 5.915 5.915 119.97 119.97 90.04 Volume: 146.39 Matrix: 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2020 0 2655 2656 3964 N (int>3sigma) = 0 0 0 0 2020 0 2569 2573 3846 Mean intensity = 0.0 0.0 0.0 0.0 29.9 0.0 75.4 78.0 76.0 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 22.9 23.0 22.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.181 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 42 42 299 883 N I>3s 42 42 286 883 0.9 0.9 0.7 35.4 9.3 9.3 5.5 26.4 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3528 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3567 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.370242 8.366805 8.361516 89.9942 90.0078 90.0104 ZERR 3.00 0.000609 0.000488 0.000607 0.0054 0.0059 0.0053 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3789250- 492069 885 883 27 32.7 1175362.80 39.14 0.045 0.061 474816- 114204 1168 1164 27 43.1 202979.52 29.84 0.051 0.064 100787- 33896 983 981 27 36.3 74629.09 16.58 0.069 0.086 9940- 1743 942 934 29 32.2 3322.14 4.53 0.167 0.210 ------------------------------------------------------------------------------------------- 3789250- 1743 3978 3962 110 36.0 340844.91 22.66 0.048 0.063 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1010 1003 27 37.1 616286.23 31.72 0.044 0.063 0.024 1.01-0.78 1219 1216 28 43.4 312884.89 21.95 0.040 0.050 0.029 0.76-0.65 1048 1047 28 37.4 235753.50 19.29 0.058 0.070 0.034 0.65-0.59 701 696 27 25.8 150848.43 15.92 0.077 0.081 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 3978 3962 110 36.0 340844.91 22.66 0.048 0.063 0.029 inf-0.60 3785 3771 99 38.1 353026.94 23.14 0.048 0.063 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1003 27 27 100.0 37.1 616286.23 216.49 0.044 0.005 1.01-0.78 1216 28 28 100.0 43.4 312884.89 154.83 0.040 0.005 0.76-0.65 1047 28 28 100.0 37.4 235753.50 125.69 0.058 0.007 0.65-0.59 696 27 27 100.0 25.8 150848.43 92.51 0.077 0.012 -------------------------------------------------------------------------------------------- inf-0.59 3962 110 110 100.0 36.0 340844.91 151.79 0.048 0.006 inf-0.60 3771 99 99 100.0 38.1 353026.94 155.96 0.048 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:25:33 2018) ID: 2932; threads 39; handles 878; mem 518404.00 (1237720.00)kB; time: 1w 5d 1h 31m 3s MEMORY INFO: Memory PF:0.0, Ph:225.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.3,peak PF: 697.1, WS: 296.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:225.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.0,peak PF: 697.1, WS: 298.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:25:33 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) 8.37024 ( 0.00061 ) 8.37691 ( 0.00061 ) 8.37554 ( 0.00049 ) 90.02113 ( 0.00533 ) 90.03240 ( 0.00536 ) 90.03043 ( 0.00588 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:25:33 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000007 0.000007 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000005 0.000005 ) M - matrix: 0.007196 -0.000001 0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007181 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000001 0.000001 0.007187 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(5) 90.021(5) 90.032(5) 90.030(6) V = 587.27(7) unit cell: 8.36620(19) 8.36620(19) 8.36620(19) 90.0 90.0 90.0 V = 585.58(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb PROFFITPEAK info: 803 peaks in the peak location table UB fit with 367 obs out of 402 (total:402,skipped:0) (91.29%) UB - matrix: -0.025182 -0.079370 -0.015604 ( 0.000030 0.000022 0.000021 ) 0.072249 -0.029478 0.032972 ( 0.000046 0.000033 0.000032 ) -0.036145 -0.003578 0.076452 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007160 -0.000002 0.000012 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007181 -0.000007 ( 0.000004 0.000004 0.000003 ) 0.000012 -0.000007 0.007176 ( 0.000004 0.000003 0.000005 ) unit cell: 8.382(4) 8.370(2) 8.373(3) 89.94(3) 90.09(3) 89.99(3) V = 587.5(4) UB fit with 367 obs out of 402 (total:402,skipped:0) (91.29%) UB - matrix: -0.025182 -0.079370 -0.015604 ( 0.000030 0.000022 0.000021 ) 0.072249 -0.029478 0.032972 ( 0.000046 0.000033 0.000032 ) -0.036145 -0.003578 0.076452 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007160 -0.000002 0.000012 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007181 -0.000007 ( 0.000004 0.000004 0.000003 ) 0.000012 -0.000007 0.007176 ( 0.000004 0.000003 0.000005 ) unit cell: 8.382(4) 8.370(2) 8.373(3) 89.94(3) 90.09(3) 89.99(3) V = 587.5(4) OTKP changes: 74 1 1 1 No constraint UB - matrix: -0.025261 -0.079113 -0.015567 ( 0.000029 0.000021 0.000020 ) 0.072050 -0.029558 0.032762 ( 0.000045 0.000032 0.000031 ) -0.035963 -0.003596 0.076251 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007123 -0.000002 0.000012 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007145 -0.000011 ( 0.000004 0.000004 0.000003 ) 0.000012 -0.000011 0.007130 ( 0.000004 0.000003 0.000005 ) Constraint UB - matrix: -0.025261 -0.079113 -0.015567 ( 0.000029 0.000021 0.000020 ) 0.072050 -0.029558 0.032762 ( 0.000045 0.000032 0.000031 ) -0.035963 -0.003596 0.076251 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007132 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007132 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007132 ( 0.000000 0.000000 0.000001 ) UB fit with 370 obs out of 402 (total:402,skipped:0) (92.04%) unit cell: 8.404(4) 8.391(2) 8.400(3) 89.91(3) 90.09(3) 89.98(3) V = 592.4(4) unit cell: 8.3985(6) 8.3985(6) 8.3985(6) 90.0 90.0 90.0 V = 592.39(7) UB fit with 370 obs out of 402 (total:402,skipped:0) (92.04%) UB - matrix: -0.025261 -0.079113 -0.015567 ( 0.000029 0.000021 0.000020 ) 0.072050 -0.029558 0.032762 ( 0.000045 0.000032 0.000031 ) -0.035963 -0.003596 0.076251 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007123 -0.000002 0.000012 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007145 -0.000011 ( 0.000004 0.000004 0.000003 ) 0.000012 -0.000011 0.007130 ( 0.000004 0.000003 0.000005 ) unit cell: 8.404(4) 8.391(2) 8.400(3) 89.91(3) 90.09(3) 89.98(3) V = 592.4(4) OTKP changes: 73 1 1 1 No constraint UB - matrix: -0.025265 -0.079085 -0.015562 ( 0.000029 0.000021 0.000020 ) 0.072032 -0.029554 0.032741 ( 0.000045 0.000032 0.000031 ) -0.035942 -0.003593 0.076238 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007119 -0.000002 0.000011 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007141 -0.000011 ( 0.000004 0.000004 0.000003 ) 0.000011 -0.000011 0.007126 ( 0.000004 0.000003 0.000005 ) Constraint UB - matrix: -0.025265 -0.079085 -0.015562 ( 0.000029 0.000021 0.000020 ) 0.072032 -0.029554 0.032741 ( 0.000045 0.000032 0.000031 ) -0.035942 -0.003593 0.076238 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007129 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007129 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007129 ( 0.000000 0.000000 0.000001 ) UB fit with 370 obs out of 402 (total:402,skipped:0) (92.04%) unit cell: 8.407(4) 8.394(2) 8.402(3) 89.91(3) 90.09(3) 89.99(3) V = 592.9(4) unit cell: 8.4009(6) 8.4009(6) 8.4009(6) 90.0 90.0 90.0 V = 592.89(8) 402 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Run 7 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=53.097) HKL list info: 579 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025265 -0.079085 -0.015562 ( 0.000029 0.000021 0.000020 ) 0.072032 -0.029554 0.032741 ( 0.000045 0.000032 0.000031 ) -0.035942 -0.003593 0.076238 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007119 -0.000002 0.000011 ( 0.000007 0.000004 0.000004 ) -0.000002 0.007141 -0.000011 ( 0.000004 0.000004 0.000003 ) 0.000011 -0.000011 0.007126 ( 0.000004 0.000003 0.000005 ) Constraint UB - matrix: -0.025265 -0.079085 -0.015562 ( 0.000029 0.000021 0.000020 ) 0.072032 -0.029554 0.032741 ( 0.000045 0.000032 0.000031 ) -0.035942 -0.003593 0.076238 ( 0.000038 0.000027 0.000026 ) M - matrix: 0.007129 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007129 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007129 ( 0.000000 0.000000 0.000001 ) UB fit with 370 obs out of 402 (total:402,skipped:0) (92.04%) unit cell: 8.407(4) 8.394(2) 8.402(3) 89.91(3) 90.09(3) 89.99(3) V = 592.9(4) unit cell: 8.4009(6) 8.4009(6) 8.4009(6) 90.0 90.0 90.0 V = 592.89(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 370 obs out of 402 (total:402,skipped:0) (92.04%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb 4 of 332 peaks identified as outliers and rejected 328 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 328 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 328 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.48 | 33 | 1.054 ( 0.178) | 1.306 ( 0.679) | 1.308 ( 0.829) | 1.42- 1.17 | 33 | 0.998 ( 0.113) | 1.064 ( 0.321) | 0.958 ( 0.451) | 1.17- 0.99 | 33 | 1.020 ( 0.094) | 1.043 ( 0.103) | 0.925 ( 0.363) | 0.99- 0.92 | 33 | 1.013 ( 0.090) | 1.012 ( 0.111) | 0.999 ( 0.349) | 0.89- 0.82 | 33 | 1.009 ( 0.090) | 1.002 ( 0.104) | 1.133 ( 0.486) | 0.82- 0.75 | 33 | 0.997 ( 0.097) | 0.956 ( 0.128) | 0.994 ( 0.379) | 0.75- 0.71 | 33 | 0.971 ( 0.057) | 0.891 ( 0.075) | 1.321 ( 0.596) | 0.71- 0.67 | 33 | 0.954 ( 0.045) | 0.858 ( 0.050) | 1.243 ( 0.513) | 0.66- 0.63 | 33 | 0.943 ( 0.045) | 0.819 ( 0.045) | 1.270 ( 0.440) | 0.63- 0.59 | 31 | 0.907 ( 0.036) | 0.766 ( 0.031) | 1.172 ( 0.452) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 328 | 0.987 ( 0.102) | 0.973 ( 0.290) | 1.132 ( 0.525) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 326 obs out of 328 (total:328,skipped:0) (99.39%) UB - matrix: -0.025265 -0.079094 -0.015656 ( 0.000017 0.000012 0.000012 ) 0.072204 -0.029558 0.032780 ( 0.000022 0.000016 0.000016 ) -0.036023 -0.003412 0.076401 ( 0.000020 0.000014 0.000014 ) M - matrix: 0.007149 -0.000013 0.000010 ( 0.000004 0.000002 0.000002 ) -0.000013 0.007141 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007157 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3888(19) 8.3936(14) 8.3844(16) 90.070(14) 90.082(17) 89.896(15) V = 590.4(2) OTKP changes: 328 1 1 1 No constraint UB - matrix: -0.025243 -0.079279 -0.015695 ( 0.000016 0.000012 0.000012 ) 0.072307 -0.029566 0.032822 ( 0.000021 0.000016 0.000016 ) -0.036142 -0.003621 0.076536 ( 0.000018 0.000014 0.000013 ) M - matrix: 0.007172 -0.000006 0.000003 ( 0.000003 0.000002 0.000002 ) -0.000006 0.007172 -0.000003 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000003 0.007181 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025243 -0.079279 -0.015695 ( 0.000016 0.000012 0.000012 ) 0.072307 -0.029566 0.032822 ( 0.000021 0.000016 0.000016 ) -0.036142 -0.003621 0.076536 ( 0.000018 0.000014 0.000013 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) unit cell: 8.3756(18) 8.3753(13) 8.3701(15) 89.974(14) 90.026(16) 89.955(15) V = 587.14(19) unit cell: 8.3736(3) 8.3736(3) 8.3736(3) 90.0 90.0 90.0 V = 587.14(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.868) HKL list info: 574 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025243 -0.079279 -0.015695 ( 0.000016 0.000012 0.000012 ) 0.072307 -0.029566 0.032822 ( 0.000021 0.000016 0.000016 ) -0.036142 -0.003621 0.076536 ( 0.000018 0.000014 0.000013 ) M - matrix: 0.007172 -0.000006 0.000003 ( 0.000003 0.000002 0.000002 ) -0.000006 0.007172 -0.000003 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000003 0.007181 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025243 -0.079279 -0.015695 ( 0.000016 0.000012 0.000012 ) 0.072307 -0.029566 0.032822 ( 0.000021 0.000016 0.000016 ) -0.036142 -0.003621 0.076536 ( 0.000018 0.000014 0.000013 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) unit cell: 8.3756(18) 8.3753(13) 8.3701(15) 89.974(14) 90.026(16) 89.955(15) V = 587.14(19) unit cell: 8.3736(3) 8.3736(3) 8.3736(3) 90.0 90.0 90.0 V = 587.14(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 328 obs out of 328 (total:328,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb 4 of 328 peaks identified as outliers and rejected 324 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 324 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 324 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 32 | 1.049 ( 0.138) | 1.260 ( 0.523) | 1.251 ( 0.736) | 1.41- 1.17 | 32 | 1.013 ( 0.109) | 1.150 ( 0.499) | 1.001 ( 0.488) | 1.17- 1.02 | 32 | 1.010 ( 0.098) | 1.035 ( 0.106) | 0.940 ( 0.376) | 0.99- 0.92 | 32 | 1.019 ( 0.089) | 1.029 ( 0.107) | 0.950 ( 0.314) | 0.92- 0.82 | 32 | 1.008 ( 0.085) | 1.010 ( 0.105) | 1.170 ( 0.503) | 0.82- 0.76 | 32 | 1.016 ( 0.099) | 0.970 ( 0.131) | 0.988 ( 0.352) | 0.75- 0.72 | 32 | 0.969 ( 0.064) | 0.902 ( 0.083) | 1.255 ( 0.544) | 0.72- 0.67 | 32 | 0.964 ( 0.046) | 0.877 ( 0.054) | 1.309 ( 0.583) | 0.67- 0.64 | 32 | 0.948 ( 0.041) | 0.825 ( 0.040) | 1.263 ( 0.442) | 0.64- 0.59 | 36 | 0.913 ( 0.041) | 0.776 ( 0.036) | 1.184 ( 0.454) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 324 | 0.990 ( 0.095) | 0.981 ( 0.279) | 1.132 ( 0.512) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.9 | 305 | 1.114 ( 0.121) | 1.236 ( 0.465) | 1.236 ( 1.042) | 12.9-18.5 | 305 | 1.075 ( 0.050) | 1.117 ( 0.213) | 1.168 ( 0.499) | 18.5-22.8 | 305 | 1.063 ( 0.073) | 1.130 ( 0.365) | 1.164 ( 0.539) | 22.9-27.1 | 305 | 1.033 ( 0.085) | 1.086 ( 0.312) | 1.130 ( 0.557) | 27.1-30.5 | 305 | 1.005 ( 0.072) | 1.007 ( 0.252) | 1.205 ( 0.498) | 30.6-33.7 | 305 | 0.973 ( 0.075) | 0.926 ( 0.093) | 1.170 ( 0.507) | 33.7-36.9 | 305 | 0.954 ( 0.070) | 0.904 ( 0.114) | 1.154 ( 0.470) | 36.9-39.7 | 305 | 0.935 ( 0.080) | 0.871 ( 0.141) | 1.214 ( 0.555) | 39.7-42.7 | 305 | 0.918 ( 0.072) | 0.836 ( 0.088) | 1.184 ( 0.535) | 42.7-50.7 | 303 | 0.920 ( 0.081) | 0.809 ( 0.065) | 1.161 ( 0.478) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3048 | 0.999 ( 0.104) | 0.992 ( 0.282) | 1.179 ( 0.591) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0020 b=1.01 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:26:11 2018 PROFFITMAIN - Started at Tue Mar 27 16:26:11 2018 OTKP changes: 3038 2 4 6 OTKP changes: 3038 2 4 6 No constraint UB - matrix: -0.025049 -0.079520 -0.015611 ( 0.000005 0.000005 0.000005 ) 0.072515 -0.029280 0.032928 ( 0.000005 0.000006 0.000006 ) -0.036236 -0.003591 0.076583 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007199 -0.000001 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007194 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000004 0.000002 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025049 -0.079520 -0.015611 ( 0.000005 0.000005 0.000005 ) 0.072515 -0.029280 0.032928 ( 0.000005 0.000006 0.000006 ) -0.036236 -0.003591 0.076583 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 3043 obs out of 3048 (total:3048,skipped:0) (99.84%) unit cell: 8.3598(5) 8.3629(5) 8.3633(4) 90.018(5) 90.030(5) 89.990(5) V = 584.70(6) unit cell: 8.36200(14) 8.36200(14) 8.36200(14) 90.0 90.0 90.0 V = 584.696(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024726 -0.079529 -0.015415 ( 0.000014 0.000011 0.000013 ) 0.072526 -0.028886 0.033053 ( 0.000012 0.000010 0.000012 ) -0.036068 -0.003519 0.076552 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007172 -0.000002 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007172 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3753(12) 8.3757(12) 8.3649(12) 90.014(11) 90.138(11) 89.987(11) V = 586.78(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007190 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3581(11) 8.3647(11) 8.3500(11) 90.050(11) 90.081(11) 89.972(11) V = 583.78(14) unit cell: 8.3576(4) 8.3576(4) 8.3576(4) 90.0 90.0 90.0 V = 583.78(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.732) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007190 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3581(11) 8.3647(11) 8.3500(11) 90.050(11) 90.081(11) 89.972(11) V = 583.78(14) unit cell: 8.3576(4) 8.3576(4) 8.3576(4) 90.0 90.0 90.0 V = 583.78(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000003 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000003 0.007190 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079634 -0.015546 ( 0.000013 0.000011 0.000013 ) 0.072648 -0.028916 0.033104 ( 0.000012 0.000010 0.000012 ) -0.036245 -0.003581 0.076670 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3581(11) 8.3647(11) 8.3500(11) 90.050(11) 90.081(11) 89.972(11) V = 583.78(14) unit cell: 8.3576(4) 8.3576(4) 8.3576(4) 90.0 90.0 90.0 V = 583.78(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024859 -0.079565 -0.015647 ( 0.000013 0.000015 0.000011 ) 0.072446 -0.029189 0.032943 ( 0.000016 0.000018 0.000013 ) -0.036283 -0.003655 0.076377 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007196 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3692(14) 8.3616(14) 8.3804(10) 90.034(12) 90.035(12) 89.967(14) V = 586.46(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024991 -0.079536 -0.015504 ( 0.000017 0.000014 0.000012 ) 0.072498 -0.029262 0.033004 ( 0.000011 0.000010 0.000008 ) -0.036257 -0.003622 0.076521 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000006 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007195 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000010 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3620(11) 8.3619(14) 8.3678(11) 89.922(12) 90.046(11) 89.981(12) V = 585.10(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007207 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007198 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3529(11) 8.3549(14) 8.3602(11) 89.934(12) 90.003(11) 89.965(12) V = 583.44(15) unit cell: 8.3560(3) 8.3560(3) 8.3560(3) 90.0 90.0 90.0 V = 583.44(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.732) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007207 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007198 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3529(11) 8.3549(14) 8.3602(11) 89.934(12) 90.003(11) 89.965(12) V = 583.44(15) unit cell: 8.3560(3) 8.3560(3) 8.3560(3) 90.0 90.0 90.0 V = 583.44(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007207 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007198 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025031 -0.079601 -0.015464 ( 0.000016 0.000014 0.000012 ) 0.072571 -0.029297 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003557 0.076618 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3529(11) 8.3549(14) 8.3602(11) 89.934(12) 90.003(11) 89.965(12) V = 583.44(15) unit cell: 8.3560(3) 8.3560(3) 8.3560(3) 90.0 90.0 90.0 V = 583.44(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025024 -0.079534 -0.015723 ( 0.000008 0.000013 0.000012 ) 0.072416 -0.029342 0.032921 ( 0.000008 0.000014 0.000014 ) -0.036202 -0.003657 0.076528 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3703(11) 8.3592(12) 8.3664(11) 90.037(11) 90.056(11) 89.983(11) V = 585.39(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007210 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3635(10) 8.3531(12) 8.3564(11) 89.995(11) 90.025(10) 90.024(11) V = 583.79(13) unit cell: 8.3577(3) 8.3577(3) 8.3577(3) 90.0 90.0 90.0 V = 583.79(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.732) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007210 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3635(10) 8.3531(12) 8.3564(11) 89.995(11) 90.025(10) 90.024(11) V = 583.79(13) unit cell: 8.3577(3) 8.3577(3) 8.3577(3) 90.0 90.0 90.0 V = 583.79(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007210 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079585 -0.015737 ( 0.000008 0.000013 0.000013 ) 0.072418 -0.029376 0.033010 ( 0.000008 0.000014 0.000013 ) -0.036320 -0.003700 0.076599 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3635(10) 8.3531(12) 8.3564(11) 89.995(11) 90.025(10) 90.024(11) V = 583.79(13) unit cell: 8.3577(3) 8.3577(3) 8.3577(3) 90.0 90.0 90.0 V = 583.79(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025241 -0.079453 -0.015762 ( 0.000011 0.000016 0.000017 ) 0.072364 -0.029417 0.032790 ( 0.000008 0.000011 0.000012 ) -0.036259 -0.003621 0.076602 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007188 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3660(10) 8.3643(14) 8.3642(11) 90.083(12) 89.946(10) 90.064(12) V = 585.28(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007201 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007209 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3576(10) 8.3584(14) 8.3537(11) 90.050(12) 89.989(10) 90.063(12) V = 583.56(14) unit cell: 8.3566(3) 8.3566(3) 8.3566(3) 90.0 90.0 90.0 V = 583.56(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.732) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007201 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007209 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3576(10) 8.3584(14) 8.3537(11) 90.050(12) 89.989(10) 90.063(12) V = 583.56(14) unit cell: 8.3566(3) 8.3566(3) 8.3566(3) 90.0 90.0 90.0 V = 583.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007201 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007209 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025247 -0.079516 -0.015751 ( 0.000011 0.000016 0.000017 ) 0.072487 -0.029415 0.032811 ( 0.000008 0.000011 0.000012 ) -0.036206 -0.003663 0.076713 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3576(10) 8.3584(14) 8.3537(11) 90.050(12) 89.989(10) 90.063(12) V = 583.56(14) unit cell: 8.3566(3) 8.3566(3) 8.3566(3) 90.0 90.0 90.0 V = 583.56(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025308 -0.079445 -0.015635 ( 0.000010 0.000008 0.000010 ) 0.072447 -0.029445 0.032793 ( 0.000014 0.000011 0.000014 ) -0.036122 -0.003534 0.076584 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000005 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000005 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007185 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3628(13) 8.3644(9) 8.3680(12) 90.047(10) 90.040(12) 90.040(10) V = 585.33(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007199 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3579(13) 8.3596(9) 8.3550(12) 90.069(10) 90.049(12) 90.027(10) V = 583.76(14) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.732) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007199 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3579(13) 8.3596(9) 8.3550(12) 90.069(10) 90.049(12) 90.027(10) V = 583.76(14) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007199 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079481 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072511 -0.029483 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076711 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3579(13) 8.3596(9) 8.3550(12) 90.069(10) 90.049(12) 90.027(10) V = 583.76(14) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.76(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 324 obs out of 324 (total:324,skipped:0) (100.00%) UB - matrix: -0.025224 -0.079284 -0.015686 ( 0.000017 0.000013 0.000013 ) 0.072354 -0.029550 0.032914 ( 0.000021 0.000016 0.000016 ) -0.036173 -0.003496 0.076579 ( 0.000020 0.000015 0.000015 ) M - matrix: 0.007180 -0.000012 0.000007 ( 0.000004 0.000002 0.000002 ) -0.000012 0.007171 0.000003 ( 0.000002 0.000002 0.000002 ) 0.000007 0.000003 0.007194 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3710(18) 8.3759(14) 8.3629(16) 90.027(15) 90.056(17) 89.907(16) V = 586.4(2) OTKP changes: 324 1 1 1 No constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007175 -0.000006 0.000003 ( 0.000003 0.000002 0.000002 ) -0.000006 0.007175 -0.000002 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000002 0.007184 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007176 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007176 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007176 ( 0.000000 0.000000 0.000001 ) UB fit with 324 obs out of 324 (total:324,skipped:0) (100.00%) unit cell: 8.3736(18) 8.3738(14) 8.3685(15) 89.983(14) 90.020(16) 89.954(15) V = 586.78(19) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.78(4) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.858) HKL list info: 566 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007175 -0.000006 0.000003 ( 0.000003 0.000002 0.000002 ) -0.000006 0.007175 -0.000002 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000002 0.007184 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007176 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007176 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007176 ( 0.000000 0.000000 0.000001 ) UB fit with 324 obs out of 324 (total:324,skipped:0) (100.00%) unit cell: 8.3736(18) 8.3738(14) 8.3685(15) 89.983(14) 90.020(16) 89.954(15) V = 586.78(19) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.78(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 324 obs out of 324 (total:324,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007175 -0.000006 0.000003 ( 0.000003 0.000002 0.000002 ) -0.000006 0.007175 -0.000002 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000002 0.007184 ( 0.000002 0.000002 0.000002 ) Constraint UB - matrix: -0.025239 -0.079295 -0.015711 ( 0.000017 0.000013 0.000013 ) 0.072322 -0.029564 0.032829 ( 0.000021 0.000015 0.000015 ) -0.036164 -0.003623 0.076547 ( 0.000018 0.000014 0.000014 ) M - matrix: 0.007176 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007176 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007176 ( 0.000000 0.000000 0.000001 ) UB fit with 324 obs out of 324 (total:324,skipped:0) (100.00%) unit cell: 8.3736(18) 8.3738(14) 8.3685(15) 89.983(14) 90.020(16) 89.954(15) V = 586.78(19) unit cell: 8.3719(4) 8.3719(4) 8.3719(4) 90.0 90.0 90.0 V = 586.78(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025052 -0.079475 -0.015592 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029292 0.032892 ( 0.000006 0.000006 0.000006 ) -0.036253 -0.003628 0.076594 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007188 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000002 0.007192 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025052 -0.079475 -0.015592 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029292 0.032892 ( 0.000006 0.000006 0.000006 ) -0.036253 -0.003628 0.076594 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) UB fit with 3043 obs out of 3048 (total:3048,skipped:0) (99.84%) unit cell: 8.3594(6) 8.3664(6) 8.3640(5) 89.983(5) 89.991(5) 89.988(5) V = 584.97(6) unit cell: 8.36328(17) 8.36328(17) 8.36328(17) 90.0 90.0 90.0 V = 584.97(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 76 reflections under beam stop or inside a detector rejection region 24 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof 4129 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:26:21 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.732) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.732) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.732) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.732) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.732) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.858) PROFFIT INFO: signal sum: min=103.0000 max=23194820.0000 PROFFIT INFO: signal sum lp corr: min=428.3857 max=3189529.8437 PROFFIT INFO: background sum: min=619.0000 max=26597.0000 PROFFIT INFO: background sum sig2: min=544.0000 max=12423.0000 PROFFIT INFO: num of signal pixels: min=50 max=546 PROFFIT INFO: Inet: min=685.4172 max=5103247.5000 PROFFIT INFO: sig(Inet): min=120.2557 max=47811.1523 PROFFIT INFO: Inet/sig(Inet): min=0.73 max=248.24 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 56 221 462 845 955 1748 2781 3798 4129 Percent 0.0 0.0 1.4 5.4 11.2 20.5 23.1 42.3 67.4 92.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4129 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4129 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5103248- 1094845 412 1825960.06 121.37 100.00 1094434- 595647 412 818654.82 101.22 100.00 594723- 253641 412 395352.35 93.10 100.00 253360- 164294 412 196486.46 70.92 100.00 164182- 115309 412 138758.55 49.46 100.00 115104- 87837 412 100647.03 35.13 100.00 87818- 61567 412 75693.07 28.26 100.00 61522- 5304 412 33966.28 18.48 100.00 5296- 2825 412 3748.74 5.16 96.12 2820- 685 421 1999.89 3.63 51.31 ------------------------------------------------------------------------------------ 5103248- 685 4129 358348.29 52.57 94.65 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 744619.06 91.45 100.00 1.41- 1.12 412 561073.69 64.31 99.27 1.12- 0.96 412 521703.55 70.58 97.09 0.96- 0.87 412 332757.83 58.40 93.69 0.87- 0.81 412 434677.79 67.56 99.27 0.81- 0.73 412 237533.43 40.59 95.63 0.73- 0.71 412 170547.36 34.16 89.32 0.71- 0.65 412 296183.98 45.84 92.96 0.65- 0.62 412 146386.92 26.49 85.68 0.62- 0.58 421 142709.88 26.85 93.59 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 358348.29 52.57 94.65 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:26:21 2018 Sorting 4129 observations 120 unique observations with > 7.00 F2/sig(F2) 4129 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 73 702 Total number of frames 702 Maximum number of 120 frame scales suggested for reliable scaling Glued frame scales: 6 frame = 1 scale 4129 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 12 120 Total number of frames 120 3311 observations > 7.00 F2/sig(F2) 3311 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 12 120 Total number of frames 120 Removing 'redundancy=1' reflections Average redundancy: 25.4 (Out of 3311 removed 4 = 3307, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3307 observations in 7 runs Run # start # end # total # 1 0 18 19 2 0 16 36 3 0 17 54 4 0 17 72 5 0 16 89 6 0 17 107 7 0 12 120 Total number of frames 120 130 unique data precomputed (should be 130) 130 unique data with 3307 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 25.4 (Out of 3307 removed 0 = 3307, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3307 observations RMS deviation of equivalent data = 0.26762 Rint = 0.20431 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20000, wR= 0.28467 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15620, wR= 0.20459, Acormin=0.562, Acormax=1.340, Acor_av=0.995 F test: Probability=1.000, F= 1.637 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13110, wR= 0.16844, Acormin=0.523, Acormax=1.437, Acor_av=0.932 F test: Probability=1.000, F= 1.418 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13202, wR= 0.17629, Acormin=0.575, Acormax=1.584, Acor_av=0.975 F test: Probability=0.000, F= 0.984 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10285, wR= 0.13854, Acormin=0.480, Acormax=1.567, Acor_av=0.923 F test: Probability=1.000, F= 1.620 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09180, wR= 0.12536, Acormin=0.462, Acormax=1.624, Acor_av=0.937 F test: Probability=1.000, F= 1.252 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11883, wR= 0.16373, Acormin=0.610, Acormax=1.640, Acor_av=0.982 F test: Probability=0.000, F= 0.596 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09326, wR= 0.12868, Acormin=0.481, Acormax=1.668, Acor_av=0.928 F test: Probability=0.000, F= 0.967 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08475, wR= 0.11791, Acormin=0.467, Acormax=1.666, Acor_av=0.938 F test: Probability=1.000, F= 1.168 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08173, wR= 0.11183, Acormin=0.319, Acormax=1.537, Acor_av=0.879 F test: Probability=0.973, F= 1.072 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11928, wR= 0.15583, Acormin=0.416, Acormax=1.431, Acor_av=0.820 F test: Probability=0.000, F= 0.470 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09257, wR= 0.12592, Acormin=0.469, Acormax=1.623, Acor_av=0.912 F test: Probability=0.000, F= 0.780 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09405, wR= 0.12372, Acormin=0.074, Acormax=0.336, Acor_av=0.180 F test: Probability=0.000, F= 0.754 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08526, wR= 0.11376, Acormin=0.070, Acormax=0.371, Acor_av=0.199 F test: Probability=0.000, F= 0.914 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07816, wR= 0.10508, Acormin=0.071, Acormax=0.397, Acor_av=0.210 F test: Probability=0.986, F= 1.082 Final absorption model (ne=6, no=5): Rint= 0.08173, Acormin=0.319, Acormax=1.537, Acor_av=0.879 Combined refinement in use Rint: 0.20442 There are 120 active scales (one needs to be fixed) Refinement control: frame scale #110 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 167 pars with 14028 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26762 Using Levenberg-Marquardt: 0.00010 New wR= 0.06791 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20431 with corrections 0.05266 Rint for all data: 0.20442 with corrections 0.05289 1 observations identified as outliers and rejected Cycle 2 wR= 0.06784 Using Levenberg-Marquardt: 0.00001 New wR= 0.06301 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20408 with corrections 0.04843 Rint for all data: 0.20442 with corrections 0.04868 0 observations identified as outliers and rejected Cycle 3 wR= 0.06301 Using Levenberg-Marquardt: 0.00000 New wR= 0.06181 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20408 with corrections 0.04773 Rint for all data: 0.20442 with corrections 0.04797 1 observations identified as outliers and rejected Cycle 4 wR= 0.06173 Using Levenberg-Marquardt: 0.00000 New wR= 0.06102 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20440 with corrections 0.04714 Rint for all data: 0.20442 with corrections 0.04762 0 observations identified as outliers and rejected Cycle 5 wR= 0.06102 Using Levenberg-Marquardt: 0.00000 New wR= 0.06065 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20440 with corrections 0.04693 Rint for all data: 0.20442 with corrections 0.04742 0 observations identified as outliers and rejected Final wR= 0.06065 Final frame scales: Min= 0.7290 Max= 1.3382 Final absorption correction factors: Amin= 0.4540 Amax= 1.5199 PROFFIT INFO: Inet (after scale3 abspack): min=692.2853 max=4424942.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=134.8739 max=53498.4102 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 4129 reflections read from tmp file 878 reflections are rejected (878 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 3 6 1 3 6 2 3 130 Initial Chi^2= 0.41466 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.86815 Current error model SIG(F2)^2 = 136.42*I_RAW + 0.00*I_BACK+(0.02147*)^2 Cycle 2, Chi^2= 0.99997 Current error model SIG(F2)^2 = 112.81*I_RAW + 0.00*I_BACK+(0.02124*)^2 Cycle 3, Chi^2= 1.00002 Current error model SIG(F2)^2 = 113.41*I_RAW + 0.00*I_BACK+(0.02110*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 113.36*I_RAW + 0.00*I_BACK+(0.02111*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 113.36*I_RAW + 0.00*I_BACK+(0.02111*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4424943- 1044630 412 1696356.30 44.14 100.00 1043495- 574204 412 774014.81 37.14 100.00 572017- 244936 412 382918.66 35.71 100.00 244889- 147349 412 182992.59 31.33 100.00 147095- 117449 412 132401.38 25.28 100.00 117261- 82781 412 96456.30 19.48 100.00 82715- 64259 412 73684.03 16.59 100.00 64227- 4710 412 36563.73 11.86 100.00 4693- 2637 412 3446.82 4.58 95.39 2635- 692 421 2022.19 3.74 71.97 ------------------------------------------------------------------------------------ 4424943- 692 4129 337353.16 22.94 96.68 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 735204.79 35.94 100.00 1.41- 1.12 412 539722.84 28.22 99.51 1.12- 0.96 412 471554.06 27.68 97.82 0.96- 0.87 412 308862.54 23.58 96.60 0.87- 0.81 412 405704.18 27.04 99.76 0.81- 0.73 412 215025.89 18.77 97.33 0.73- 0.71 412 161863.15 17.57 91.99 0.71- 0.65 412 273876.78 21.79 97.33 0.65- 0.62 412 136158.65 14.25 90.53 0.62- 0.58 421 130086.42 14.76 95.96 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 337353.16 22.94 96.68 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 735204.79 35.94 100.00 4.82- 1.12 824 637463.82 32.08 99.76 4.82- 0.96 1236 582160.56 30.62 99.11 4.82- 0.87 1648 513836.06 28.86 98.48 4.82- 0.81 2060 492209.68 28.49 98.74 4.82- 0.73 2472 446012.38 26.87 98.50 4.82- 0.71 2884 405419.64 25.54 97.57 4.82- 0.65 3296 388976.78 25.07 97.54 4.82- 0.62 3708 360885.87 23.87 96.76 4.82- 0.58 4129 337353.16 22.94 96.68 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 337353.16 22.94 96.68 Scale applied to data: s=0.225991 (maximum obs:4424942.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.028: data 4129 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.028: data 4115 -> merged 157 Rejected total: 14, method kkm 11, method Blessing 3 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585547, 4.828542 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.48 14 14 24.36 100.00 341 1.41 - 1.12 14 14 34.00 100.00 476 1.12 - 0.97 14 14 33.86 100.00 474 0.96 - 0.84 14 14 35.79 100.00 501 0.84 - 0.78 14 14 27.79 100.00 389 0.78 - 0.73 14 14 29.07 100.00 407 0.73 - 0.69 14 14 26.93 100.00 377 0.69 - 0.66 14 14 23.00 100.00 322 0.65 - 0.63 14 14 24.14 100.00 338 0.63 - 0.60 14 14 21.14 100.00 296 --------------------------------------------------------------- 8.37 - 0.60 140 140 28.01 100.00 3921 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:26:22 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.359384 8.366430 8.364030 89.9826 89.9908 89.9884 4115 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2099 0 2765 2760 4115 N (int>3sigma) = 0 0 0 0 2099 0 2674 2667 3978 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.4 78.4 76.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 23.0 23.1 22.9 Lattice type: F chosen Volume: 584.97 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.913 5.913 119.97 90.03 119.98 Niggli form: a.a = 34.953 b.b = 34.962 c.c = 34.965 b.c = -17.464 a.c = -0.019 a.b = -17.469 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.027 CUBIC F-lattice R(int) = 0.047 [ 3958] Vol = 585.0 Cell: 8.359 8.366 8.364 90.02 89.99 90.01 Volume: 584.97 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.027 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 3674] Vol = 438.7 Cell: 5.913 5.912 14.489 89.97 90.04 119.98 Volume: 438.72 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.027 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1163] Vol = 438.7 Trigonal Cell: 5.913 5.912 14.489 89.97 90.04 119.98 Volume: 438.72 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.028 TETRAGONAL I-lattice R(int) = 0.045 [ 3708] Vol = 292.5 Cell: 5.914 5.916 8.359 89.99 90.00 90.02 Volume: 292.48 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.025 TETRAGONAL I-lattice R(int) = 0.045 [ 3708] Vol = 292.5 Cell: 5.914 5.916 8.359 89.99 90.00 90.02 Volume: 292.48 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3654] Vol = 292.5 Cell: 5.914 8.359 5.916 89.99 89.98 90.00 Volume: 292.48 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.044 [ 3300] Vol = 292.5 Cell: 8.359 5.914 5.916 90.02 90.01 90.00 Volume: 292.48 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.021 MONOCLINIC I-lattice R(int) = 0.043 [ 3298] Vol = 292.5 Cell: 5.913 5.912 8.366 90.00 90.02 89.97 Volume: 292.48 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.016 MONOCLINIC C-lattice R(int) = 0.044 [ 3312] Vol = 292.5 Cell: 8.359 8.366 5.912 90.00 134.98 90.01 Volume: 292.48 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2624] Vol = 146.2 Cell: 5.912 5.913 5.913 119.97 90.03 119.98 Volume: 146.24 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2099 0 2756 2775 4115 N (int>3sigma) = 0 0 0 0 2099 0 2662 2681 3978 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.8 77.2 76.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 23.0 23.0 22.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.170 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 317 918 N I>3s 45 45 299 918 0.9 0.9 0.7 35.8 8.9 8.9 5.4 26.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3661 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3700 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359384 8.366430 8.364030 90.0174 89.9908 90.0116 ZERR 3.00 0.000577 0.000566 0.000457 0.0050 0.0051 0.0055 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3758573- 710572 674 672 26 25.8 1361803.34 41.83 0.041 0.053 701517- 213415 638 635 26 24.4 426338.16 35.76 0.059 0.074 208558- 92553 957 957 26 36.8 140682.55 25.98 0.046 0.059 89149- 63616 673 671 26 25.8 77281.40 16.85 0.069 0.088 61037- 3321 524 520 26 20.0 23358.54 8.87 0.086 0.117 3246- 1675 663 660 27 24.4 2522.14 4.25 0.203 0.265 ------------------------------------------------------------------------------------------- 3758573- 1675 4129 4115 157 26.2 336854.59 22.94 0.047 0.060 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 779 773 26 29.7 586247.11 31.42 0.044 0.056 0.023 1.12-0.88 910 908 26 34.9 435151.08 26.69 0.036 0.048 0.026 0.85-0.75 762 762 26 29.3 309197.33 22.35 0.046 0.058 0.029 0.74-0.68 670 669 26 25.7 244387.44 20.13 0.059 0.071 0.033 0.67-0.63 632 631 26 24.3 139536.00 15.81 0.072 0.089 0.042 0.62-0.59 376 372 27 13.8 136343.15 14.54 0.073 0.075 0.043 ------------------------------------------------------------------------------------------------------ inf-0.59 4129 4115 157 26.2 336854.59 22.94 0.047 0.060 0.028 inf-0.60 3930 3919 139 28.2 348840.68 23.42 0.046 0.060 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 773 26 26 100.0 29.7 586247.11 185.88 0.044 0.005 1.12-0.88 908 26 26 100.0 34.9 435151.08 160.50 0.036 0.005 0.85-0.75 762 26 26 100.0 29.3 309197.33 127.68 0.046 0.005 0.74-0.68 669 26 26 100.0 25.7 244387.44 104.14 0.059 0.007 0.67-0.63 631 26 26 100.0 24.3 139536.00 77.15 0.072 0.009 0.62-0.59 372 27 27 100.0 13.8 136343.15 61.97 0.073 0.015 -------------------------------------------------------------------------------------------- inf-0.59 4115 157 157 100.0 26.2 336854.59 128.34 0.047 0.006 inf-0.60 3919 139 139 100.0 28.2 348840.68 132.24 0.046 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025052 -0.079475 -0.015592 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029292 0.032892 ( 0.000006 0.000006 0.000006 ) -0.036253 -0.003628 0.076594 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007187 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000002 0.007192 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025052 -0.079475 -0.015592 ( 0.000006 0.000006 0.000006 ) 0.072510 -0.029292 0.032892 ( 0.000006 0.000006 0.000006 ) -0.036253 -0.003628 0.076594 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3594(6) 8.3665(6) 8.3640(5) 89.983(5) 89.991(5) 89.989(5) V = 584.97(6) unit cell: 8.36329(17) 8.36329(17) 8.36329(17) 90.0 90.0 90.0 V = 584.97(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.732) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.732) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.732) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.732) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.732) Run 7 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.858) PROFFIT INFO: signal sum: min=103.0000 max=23194820.0000 PROFFIT INFO: signal sum lp corr: min=428.3857 max=3189529.8437 PROFFIT INFO: background sum: min=619.0000 max=26597.0000 PROFFIT INFO: background sum sig2: min=544.0000 max=12423.0000 PROFFIT INFO: num of signal pixels: min=50 max=546 PROFFIT INFO: Inet: min=685.4172 max=5103247.5000 PROFFIT INFO: sig(Inet): min=120.2557 max=47811.1523 PROFFIT INFO: Inet/sig(Inet): min=0.73 max=248.24 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 112 442 924 1690 1910 3496 5562 7596 8258 Percent 0.0 0.0 1.4 5.4 11.2 20.5 23.1 42.3 67.4 92.0 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4129 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4129 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5103248- 1094845 412 1825960.06 121.37 100.00 1094434- 595647 412 818654.82 101.22 100.00 594723- 253641 412 395352.35 93.10 100.00 253360- 164294 412 196486.46 70.92 100.00 164182- 115309 412 138758.55 49.46 100.00 115104- 87837 412 100647.03 35.13 100.00 87818- 61567 412 75693.07 28.26 100.00 61522- 5304 412 33966.28 18.48 100.00 5296- 2825 412 3748.74 5.16 96.12 2820- 685 421 1999.89 3.63 51.31 ------------------------------------------------------------------------------------ 5103248- 685 4129 358348.29 52.57 94.65 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 744619.06 91.45 100.00 1.41- 1.12 412 561073.69 64.31 99.27 1.12- 0.96 412 521703.55 70.58 97.09 0.96- 0.87 412 332757.83 58.40 93.69 0.87- 0.81 412 434677.79 67.56 99.27 0.81- 0.73 412 237533.43 40.59 95.63 0.73- 0.71 412 170547.36 34.16 89.32 0.71- 0.65 412 296183.98 45.84 92.96 0.65- 0.62 412 146386.92 26.49 85.68 0.62- 0.58 421 142709.88 26.85 93.59 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 358348.29 52.57 94.65 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:26:23 2018 Sorting 4129 observations 85 unique observations with > 7.00 F2/sig(F2) 4129 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 73 702 Total number of frames 702 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4129 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 8 80 Total number of frames 80 3311 observations > 7.00 F2/sig(F2) 3311 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 8 80 Total number of frames 80 Removing 'redundancy=1' reflections Average redundancy: 35.6 (Out of 3311 removed 4 = 3307, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3307 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 8 80 Total number of frames 80 93 unique data precomputed (should be 93) 93 unique data with 3307 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 35.6 (Out of 3307 removed 0 = 3307, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3307 observations RMS deviation of equivalent data = 0.26830 Rint = 0.20460 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20014, wR= 0.28526 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15649, wR= 0.20512, Acormin=0.562, Acormax=1.340, Acor_av=0.995 F test: Probability=1.000, F= 1.633 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13138, wR= 0.16893, Acormin=0.523, Acormax=1.436, Acor_av=0.932 F test: Probability=1.000, F= 1.417 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13222, wR= 0.17672, Acormin=0.577, Acormax=1.586, Acor_av=0.975 F test: Probability=0.000, F= 0.985 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10296, wR= 0.13896, Acormin=0.479, Acormax=1.569, Acor_av=0.923 F test: Probability=1.000, F= 1.624 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09197, wR= 0.12593, Acormin=0.459, Acormax=1.626, Acor_av=0.937 F test: Probability=1.000, F= 1.250 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11879, wR= 0.16418, Acormin=0.610, Acormax=1.647, Acor_av=0.984 F test: Probability=0.000, F= 0.599 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09350, wR= 0.12910, Acormin=0.482, Acormax=1.665, Acor_av=0.930 F test: Probability=0.000, F= 0.966 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08488, wR= 0.11842, Acormin=0.468, Acormax=1.674, Acor_av=0.939 F test: Probability=1.000, F= 1.169 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08204, wR= 0.11237, Acormin=0.320, Acormax=1.539, Acor_av=0.880 F test: Probability=0.965, F= 1.067 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11930, wR= 0.15633, Acormin=0.420, Acormax=1.426, Acor_av=0.822 F test: Probability=0.000, F= 0.474 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09268, wR= 0.12630, Acormin=0.473, Acormax=1.620, Acor_av=0.913 F test: Probability=0.000, F= 0.784 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09442, wR= 0.12466, Acormin=0.073, Acormax=0.333, Acor_av=0.177 F test: Probability=0.000, F= 0.754 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08576, wR= 0.11486, Acormin=0.070, Acormax=0.366, Acor_av=0.196 F test: Probability=0.000, F= 0.910 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07852, wR= 0.10591, Acormin=0.070, Acormax=0.391, Acor_av=0.206 F test: Probability=0.985, F= 1.081 Final absorption model (ne=6, no=5): Rint= 0.08204, Acormin=0.320, Acormax=1.539, Acor_av=0.880 Combined refinement in use Rint: 0.20471 There are 80 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 127 pars with 8128 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26830 Using Levenberg-Marquardt: 0.00010 New wR= 0.07174 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20460 with corrections 0.05601 Rint for all data: 0.20471 with corrections 0.05624 1 observations identified as outliers and rejected Cycle 2 wR= 0.07168 Using Levenberg-Marquardt: 0.00001 New wR= 0.06651 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20437 with corrections 0.05141 Rint for all data: 0.20471 with corrections 0.05168 0 observations identified as outliers and rejected Cycle 3 wR= 0.06651 Using Levenberg-Marquardt: 0.00000 New wR= 0.06470 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20437 with corrections 0.05013 Rint for all data: 0.20471 with corrections 0.05038 0 observations identified as outliers and rejected Cycle 4 wR= 0.06470 Using Levenberg-Marquardt: 0.00000 New wR= 0.06360 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20437 with corrections 0.04937 Rint for all data: 0.20471 with corrections 0.04961 0 observations identified as outliers and rejected Cycle 5 wR= 0.06360 Using Levenberg-Marquardt: 0.00000 New wR= 0.06284 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20437 with corrections 0.04886 Rint for all data: 0.20471 with corrections 0.04910 1 observations identified as outliers and rejected Final wR= 0.06284 Final frame scales: Min= 0.7949 Max= 1.2996 Final absorption correction factors: Amin= 0.4573 Amax= 1.4520 PROFFIT INFO: Inet (after scale3 abspack): min=710.3943 max=4468929.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=133.1907 max=52870.0469 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 4129 reflections read from tmp file 931 reflections are rejected (930 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 2 4 1 2 2 1 3 94 Initial Chi^2= 0.40213 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.93507 Current error model SIG(F2)^2 = 144.30*I_RAW + 0.00*I_BACK+(0.01829*)^2 Cycle 2, Chi^2= 1.00488 Current error model SIG(F2)^2 = 106.42*I_RAW + 0.00*I_BACK+(0.02268*)^2 Cycle 3, Chi^2= 1.00018 Current error model SIG(F2)^2 = 111.57*I_RAW + 0.00*I_BACK+(0.02173*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 111.15*I_RAW + 0.00*I_BACK+(0.02183*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 111.15*I_RAW + 0.00*I_BACK+(0.02183*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4468930- 1044975 412 1691388.30 42.99 100.00 1040612- 577855 412 774548.34 36.55 100.00 576803- 244128 412 382834.91 35.13 100.00 244016- 146301 412 182767.49 30.95 100.00 146235- 117399 412 132568.87 25.19 100.00 117397- 83236 412 96390.58 19.45 100.00 83219- 64220 412 73974.55 16.74 100.00 63956- 4686 412 36645.28 11.90 100.00 4682- 2628 412 3452.55 4.61 96.12 2626- 710 421 2021.56 3.80 72.92 ------------------------------------------------------------------------------------ 4468930- 710 4129 336927.65 22.69 96.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 731383.71 35.15 100.00 1.41- 1.12 412 538509.87 27.77 99.51 1.12- 0.96 412 470538.81 27.29 97.82 0.96- 0.87 412 308986.78 23.32 96.84 0.87- 0.81 412 405553.74 26.72 99.76 0.81- 0.73 412 215295.41 18.65 97.57 0.73- 0.71 412 161833.96 17.53 92.23 0.71- 0.65 412 274566.75 21.65 97.33 0.65- 0.62 412 136716.27 14.23 91.26 0.62- 0.58 421 130402.68 14.75 96.20 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 336927.65 22.69 96.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 412 731383.71 35.15 100.00 4.82- 1.12 824 634946.79 31.46 99.76 4.82- 0.96 1236 580144.13 30.07 99.11 4.82- 0.87 1648 512354.79 28.38 98.54 4.82- 0.81 2060 490994.58 28.05 98.79 4.82- 0.73 2472 445044.72 26.48 98.58 4.82- 0.71 2884 404586.04 25.20 97.68 4.82- 0.65 3296 388333.63 24.76 97.63 4.82- 0.62 3708 360376.14 23.59 96.93 4.82- 0.58 4129 336927.65 22.69 96.85 ------------------------------------------------------------------------------------ 4.82- 0.58 4129 336927.65 22.69 96.85 Scale applied to data: s=0.223767 (maximum obs:4468929.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.049; Rsigma 0.029: data 4129 -> merged 110 With outlier rejection... Rint 0.048; Rsigma 0.029: data 4112 -> merged 110 Rejected total: 17, method kkm 14, method Blessing 3 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585548, 4.828549 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.37 - 1.71 10 10 25.90 100.00 259 1.61 - 1.21 10 10 38.10 100.00 381 1.17 - 1.01 10 10 49.00 100.00 490 0.99 - 0.89 10 10 47.50 100.00 475 0.88 - 0.81 10 10 45.50 100.00 455 0.81 - 0.74 10 10 39.80 100.00 398 0.73 - 0.71 10 10 43.60 100.00 436 0.70 - 0.66 10 10 36.10 100.00 361 0.66 - 0.64 10 10 34.20 100.00 342 0.63 - 0.60 10 10 32.00 100.00 320 --------------------------------------------------------------- 8.37 - 0.60 100 100 39.17 100.00 3917 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:26:22 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.359384 8.366430 8.364030 89.9826 89.9908 89.9884 4115 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.94 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2099 0 2765 2760 4115 N (int>3sigma) = 0 0 0 0 2099 0 2674 2667 3978 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.4 78.4 76.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 23.0 23.1 22.9 Lattice type: F chosen Volume: 584.97 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.913 5.913 119.97 90.03 119.98 Niggli form: a.a = 34.953 b.b = 34.962 c.c = 34.965 b.c = -17.464 a.c = -0.019 a.b = -17.469 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.027 CUBIC F-lattice R(int) = 0.047 [ 3958] Vol = 585.0 Cell: 8.359 8.366 8.364 90.02 89.99 90.01 Volume: 584.97 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.027 RHOMBOHEDRAL R-lattice R(int) = 0.051 [ 3674] Vol = 438.7 Cell: 5.913 5.912 14.489 89.97 90.04 119.98 Volume: 438.72 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.027 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1163] Vol = 438.7 Trigonal Cell: 5.913 5.912 14.489 89.97 90.04 119.98 Volume: 438.72 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.028 TETRAGONAL I-lattice R(int) = 0.045 [ 3708] Vol = 292.5 Cell: 5.914 5.916 8.359 89.99 90.00 90.02 Volume: 292.48 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.025 TETRAGONAL I-lattice R(int) = 0.045 [ 3708] Vol = 292.5 Cell: 5.914 5.916 8.359 89.99 90.00 90.02 Volume: 292.48 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3654] Vol = 292.5 Cell: 5.914 8.359 5.916 89.99 89.98 90.00 Volume: 292.48 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.010 MONOCLINIC I-lattice R(int) = 0.044 [ 3300] Vol = 292.5 Cell: 8.359 5.914 5.916 90.02 90.01 90.00 Volume: 292.48 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.021 MONOCLINIC I-lattice R(int) = 0.043 [ 3298] Vol = 292.5 Cell: 5.913 5.912 8.366 90.00 90.02 89.97 Volume: 292.48 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.016 MONOCLINIC C-lattice R(int) = 0.044 [ 3312] Vol = 292.5 Cell: 8.359 8.366 5.912 90.00 134.98 90.01 Volume: 292.48 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2624] Vol = 146.2 Cell: 5.912 5.913 5.913 119.97 90.03 119.98 Volume: 146.24 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2099 0 2756 2775 4115 N (int>3sigma) = 0 0 0 0 2099 0 2662 2681 3978 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 75.8 77.2 76.1 Mean int/sigma = 0.0 0.0 0.0 0.0 23.8 0.0 23.0 23.0 22.9 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.170 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 317 918 N I>3s 45 45 299 918 0.9 0.9 0.7 35.8 8.9 8.9 5.4 26.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3661 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3700 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359384 8.366430 8.364030 90.0174 89.9908 90.0116 ZERR 3.00 0.000577 0.000566 0.000457 0.0050 0.0051 0.0055 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3740659- 491848 918 915 27 33.9 1158794.41 38.91 0.045 0.058 471716- 113132 1217 1213 27 44.9 201712.93 29.86 0.053 0.066 100395- 33431 1020 1018 27 37.7 74338.68 16.71 0.068 0.087 9847- 1744 974 966 29 33.3 3293.37 4.59 0.170 0.215 ------------------------------------------------------------------------------------------- 3740659- 1744 4129 4112 110 37.4 336535.22 22.68 0.048 0.061 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1053 1045 27 38.7 602818.91 31.63 0.043 0.058 0.024 1.01-0.78 1263 1260 28 45.0 310355.26 21.96 0.042 0.052 0.029 0.76-0.65 1089 1088 28 38.9 232729.66 19.28 0.058 0.069 0.034 0.65-0.59 724 719 27 26.6 152475.07 16.10 0.075 0.081 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 4129 4112 110 37.4 336535.22 22.68 0.048 0.061 0.029 inf-0.60 3930 3915 99 39.5 348493.92 23.15 0.048 0.060 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1045 27 27 100.0 38.7 602818.91 220.57 0.043 0.005 1.01-0.78 1260 28 28 100.0 45.0 310355.26 157.63 0.042 0.005 0.76-0.65 1088 28 28 100.0 38.9 232729.66 127.75 0.058 0.006 0.65-0.59 719 27 27 100.0 26.6 152475.07 96.04 0.075 0.011 -------------------------------------------------------------------------------------------- inf-0.59 4112 110 110 100.0 37.4 336535.22 154.95 0.048 0.006 inf-0.60 3915 99 99 100.0 39.5 348493.92 159.15 0.048 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:30:38 2018) ID: 2932; threads 39; handles 878; mem 518920.00 (1237720.00)kB; time: 1w 5d 1h 36m 9s MEMORY INFO: Memory PF:0.0, Ph:223.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.8,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:223.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.5,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:30:39 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) 8.37024 ( 0.00058 ) 8.37691 ( 0.00057 ) 8.37554 ( 0.00046 ) 90.02113 ( 0.00497 ) 90.03240 ( 0.00506 ) 90.03043 ( 0.00553 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:30:39 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000006 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000001 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000001 0.007187 -0.000002 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000002 0.007192 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(5) 90.021(5) 90.032(5) 90.030(5) V = 587.27(6) unit cell: 8.36329(17) 8.36329(17) 8.36329(17) 90.0 90.0 90.0 V = 584.97(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 453 peaks identified as outliers and rejected 446 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 446 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 446 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.78 | 45 | 1.102 ( 0.098) | 1.019 ( 0.122) | 1.365 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.985 ( 0.124) | 1.369 ( 0.513) | 0.73- 0.69 | 45 | 1.088 ( 0.080) | 0.931 ( 0.104) | 1.361 ( 0.510) | 0.69- 0.66 | 45 | 1.068 ( 0.074) | 0.886 ( 0.097) | 1.333 ( 0.455) | 0.65- 0.62 | 45 | 1.047 ( 0.075) | 0.849 ( 0.050) | 1.363 ( 0.607) | 0.62- 0.59 | 41 | 1.026 ( 0.086) | 0.808 ( 0.035) | 1.416 ( 0.564) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 446 | 1.062 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.880) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 445 obs out of 446 (total:446,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072471 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036035 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 445 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.078(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.078(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 446 (total:446,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.477) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.870 ( 0.063) | 1.446 ( 0.588) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.286 ( 0.496) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=67, end=91, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_7_67.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_67.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_7_67.rpb PROFFITPEAK info: 959 peaks in the peak location table UB fit with 438 obs out of 484 (total:484,skipped:0) (90.50%) UB - matrix: -0.025206 -0.079368 -0.015590 ( 0.000028 0.000020 0.000020 ) 0.072304 -0.029479 0.032928 ( 0.000042 0.000030 0.000030 ) -0.036165 -0.003582 0.076471 ( 0.000032 0.000023 0.000023 ) M - matrix: 0.007171 -0.000001 0.000008 ( 0.000007 0.000003 0.000004 ) -0.000001 0.007181 -0.000007 ( 0.000003 0.000004 0.000003 ) 0.000008 -0.000007 0.007175 ( 0.000004 0.000003 0.000004 ) unit cell: 8.376(3) 8.370(2) 8.374(3) 89.94(2) 90.07(3) 89.99(3) V = 587.1(3) UB fit with 438 obs out of 484 (total:484,skipped:0) (90.50%) UB - matrix: -0.025206 -0.079368 -0.015590 ( 0.000028 0.000020 0.000020 ) 0.072304 -0.029479 0.032928 ( 0.000042 0.000030 0.000030 ) -0.036165 -0.003582 0.076471 ( 0.000032 0.000023 0.000023 ) M - matrix: 0.007171 -0.000001 0.000008 ( 0.000007 0.000003 0.000004 ) -0.000001 0.007181 -0.000007 ( 0.000003 0.000004 0.000003 ) 0.000008 -0.000007 0.007175 ( 0.000004 0.000003 0.000004 ) unit cell: 8.376(3) 8.370(2) 8.374(3) 89.94(2) 90.07(3) 89.99(3) V = 587.1(3) OTKP changes: 90 1 1 1 No constraint UB - matrix: -0.025265 -0.079128 -0.015560 ( 0.000026 0.000019 0.000019 ) 0.072129 -0.029564 0.032758 ( 0.000039 0.000028 0.000028 ) -0.036000 -0.003570 0.076295 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007137 -0.000005 0.000009 ( 0.000006 0.000003 0.000004 ) -0.000005 0.007148 -0.000010 ( 0.000003 0.000003 0.000003 ) 0.000009 -0.000010 0.007136 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025265 -0.079128 -0.015560 ( 0.000026 0.000019 0.000019 ) 0.072129 -0.029564 0.032758 ( 0.000039 0.000028 0.000028 ) -0.036000 -0.003570 0.076295 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007137 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007137 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007137 ( 0.000000 0.000000 0.000001 ) UB fit with 439 obs out of 484 (total:484,skipped:0) (90.70%) unit cell: 8.396(3) 8.390(2) 8.397(3) 89.92(2) 90.07(3) 89.96(3) V = 591.4(3) unit cell: 8.3940(6) 8.3940(6) 8.3940(6) 90.0 90.0 90.0 V = 591.44(7) UB fit with 439 obs out of 484 (total:484,skipped:0) (90.70%) UB - matrix: -0.025265 -0.079128 -0.015560 ( 0.000026 0.000019 0.000019 ) 0.072129 -0.029564 0.032758 ( 0.000039 0.000028 0.000028 ) -0.036000 -0.003570 0.076295 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007137 -0.000005 0.000009 ( 0.000006 0.000003 0.000004 ) -0.000005 0.007148 -0.000010 ( 0.000003 0.000003 0.000003 ) 0.000009 -0.000010 0.007136 ( 0.000004 0.000003 0.000004 ) unit cell: 8.396(3) 8.390(2) 8.397(3) 89.92(2) 90.07(3) 89.96(3) V = 591.4(3) OTKP changes: 89 1 1 1 No constraint UB - matrix: -0.025270 -0.079101 -0.015553 ( 0.000026 0.000019 0.000019 ) 0.072112 -0.029561 0.032739 ( 0.000039 0.000028 0.000028 ) -0.035979 -0.003566 0.076281 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007133 -0.000005 0.000009 ( 0.000006 0.000003 0.000004 ) -0.000005 0.007144 -0.000010 ( 0.000003 0.000003 0.000003 ) 0.000009 -0.000010 0.007132 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025270 -0.079101 -0.015553 ( 0.000026 0.000019 0.000019 ) 0.072112 -0.029561 0.032739 ( 0.000039 0.000028 0.000028 ) -0.035979 -0.003566 0.076281 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007134 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007134 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007134 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 484 (total:484,skipped:0) (90.91%) unit cell: 8.398(3) 8.392(2) 8.399(3) 89.92(2) 90.07(3) 89.96(3) V = 591.9(3) unit cell: 8.3963(6) 8.3963(6) 8.3963(6) 90.0 90.0 90.0 V = 591.93(7) 484 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=53.070) HKL list info: 679 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025270 -0.079101 -0.015553 ( 0.000026 0.000019 0.000019 ) 0.072112 -0.029561 0.032739 ( 0.000039 0.000028 0.000028 ) -0.035979 -0.003566 0.076281 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007133 -0.000005 0.000009 ( 0.000006 0.000003 0.000004 ) -0.000005 0.007144 -0.000010 ( 0.000003 0.000003 0.000003 ) 0.000009 -0.000010 0.007132 ( 0.000004 0.000003 0.000004 ) Constraint UB - matrix: -0.025270 -0.079101 -0.015553 ( 0.000026 0.000019 0.000019 ) 0.072112 -0.029561 0.032739 ( 0.000039 0.000028 0.000028 ) -0.035979 -0.003566 0.076281 ( 0.000033 0.000024 0.000024 ) M - matrix: 0.007134 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007134 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007134 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 484 (total:484,skipped:0) (90.91%) unit cell: 8.398(3) 8.392(2) 8.399(3) 89.92(2) 90.07(3) 89.96(3) V = 591.9(3) unit cell: 8.3963(6) 8.3963(6) 8.3963(6) 90.0 90.0 90.0 V = 591.93(7) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 439 obs out of 484 (total:484,skipped:0) (90.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=67, end=91, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_67.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_67.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_67.rpb 7 of 404 peaks identified as outliers and rejected 397 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 397 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 397 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.48 | 40 | 1.021 ( 0.096) | 1.226 ( 0.499) | 1.167 ( 0.725) | 1.42- 1.17 | 40 | 1.016 ( 0.111) | 1.118 ( 0.417) | 1.025 ( 0.482) | 1.17- 0.99 | 40 | 1.022 ( 0.092) | 1.043 ( 0.107) | 0.938 ( 0.357) | 0.99- 0.88 | 40 | 1.020 ( 0.092) | 1.009 ( 0.114) | 1.036 ( 0.353) | 0.88- 0.82 | 40 | 1.007 ( 0.089) | 0.998 ( 0.111) | 1.131 ( 0.485) | 0.82- 0.74 | 40 | 0.995 ( 0.093) | 0.958 ( 0.130) | 1.056 ( 0.404) | 0.74- 0.71 | 40 | 0.975 ( 0.057) | 0.895 ( 0.069) | 1.272 ( 0.574) | 0.71- 0.67 | 40 | 0.955 ( 0.044) | 0.859 ( 0.050) | 1.241 ( 0.512) | 0.66- 0.63 | 40 | 0.944 ( 0.042) | 0.826 ( 0.045) | 1.222 ( 0.425) | 0.63- 0.59 | 37 | 0.903 ( 0.035) | 0.770 ( 0.034) | 1.139 ( 0.406) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 397 | 0.986 ( 0.088) | 0.972 ( 0.257) | 1.123 ( 0.496) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 395 obs out of 397 (total:397,skipped:0) (99.50%) UB - matrix: -0.025253 -0.079109 -0.015663 ( 0.000013 0.000010 0.000011 ) 0.072227 -0.029530 0.032796 ( 0.000018 0.000014 0.000015 ) -0.036051 -0.003414 0.076453 ( 0.000017 0.000013 0.000014 ) M - matrix: 0.007154 -0.000012 0.000008 ( 0.000003 0.000002 0.000002 ) -0.000012 0.007142 0.000010 ( 0.000002 0.000002 0.000001 ) 0.000008 0.000010 0.007166 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3859(16) 8.3931(12) 8.3790(14) 90.077(13) 90.065(15) 89.903(13) V = 589.75(17) OTKP changes: 397 1 1 1 No constraint UB - matrix: -0.025232 -0.079286 -0.015696 ( 0.000013 0.000010 0.000010 ) 0.072288 -0.029548 0.032814 ( 0.000017 0.000014 0.000014 ) -0.036147 -0.003628 0.076537 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007169 -0.000004 0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007173 -0.000003 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000003 0.007181 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025232 -0.079286 -0.015696 ( 0.000013 0.000010 0.000010 ) 0.072288 -0.029548 0.032814 ( 0.000017 0.000014 0.000014 ) -0.036147 -0.003628 0.076537 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 397 obs out of 397 (total:397,skipped:0) (100.00%) unit cell: 8.3773(15) 8.3752(11) 8.3702(13) 89.978(12) 90.012(14) 89.966(13) V = 587.27(16) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) *** 3D peak analysis started - run 7 (2nd cycle) *** Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.874) HKL list info: 674 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025232 -0.079286 -0.015696 ( 0.000013 0.000010 0.000010 ) 0.072288 -0.029548 0.032814 ( 0.000017 0.000014 0.000014 ) -0.036147 -0.003628 0.076537 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007169 -0.000004 0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007173 -0.000003 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000003 0.007181 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025232 -0.079286 -0.015696 ( 0.000013 0.000010 0.000010 ) 0.072288 -0.029548 0.032814 ( 0.000017 0.000014 0.000014 ) -0.036147 -0.003628 0.076537 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007173 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007173 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007173 ( 0.000000 0.000000 0.000001 ) UB fit with 397 obs out of 397 (total:397,skipped:0) (100.00%) unit cell: 8.3773(15) 8.3752(11) 8.3702(13) 89.978(12) 90.012(14) 89.966(13) V = 587.27(16) unit cell: 8.3742(3) 8.3742(3) 8.3742(3) 90.0 90.0 90.0 V = 587.27(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 397 obs out of 397 (total:397,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=67, end=91, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_67.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_67.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_67.rpb 7 of 401 peaks identified as outliers and rejected 394 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" 394 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7.tabbin file 394 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_7.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 39 | 1.034 ( 0.140) | 1.212 ( 0.488) | 1.144 ( 0.710) | 1.41- 1.17 | 39 | 1.017 ( 0.109) | 1.175 ( 0.516) | 1.084 ( 0.530) | 1.17- 0.99 | 39 | 1.025 ( 0.094) | 1.047 ( 0.109) | 0.944 ( 0.361) | 0.99- 0.89 | 39 | 1.018 ( 0.096) | 1.012 ( 0.121) | 1.026 ( 0.379) | 0.89- 0.82 | 39 | 1.019 ( 0.086) | 1.008 ( 0.096) | 1.145 ( 0.483) | 0.82- 0.75 | 39 | 1.007 ( 0.087) | 0.964 ( 0.126) | 1.064 ( 0.402) | 0.75- 0.71 | 39 | 0.968 ( 0.066) | 0.899 ( 0.082) | 1.221 ( 0.547) | 0.71- 0.67 | 39 | 0.965 ( 0.044) | 0.877 ( 0.053) | 1.246 ( 0.535) | 0.67- 0.63 | 39 | 0.948 ( 0.039) | 0.830 ( 0.043) | 1.280 ( 0.452) | 0.63- 0.59 | 43 | 0.909 ( 0.040) | 0.782 ( 0.038) | 1.129 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 394 | 0.990 ( 0.094) | 0.978 ( 0.273) | 1.128 ( 0.501) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.8 | 312 | 1.115 ( 0.120) | 1.240 ( 0.472) | 1.237 ( 1.033) | 12.9-18.5 | 312 | 1.075 ( 0.050) | 1.116 ( 0.211) | 1.171 ( 0.499) | 18.5-22.9 | 312 | 1.063 ( 0.072) | 1.129 ( 0.361) | 1.162 ( 0.537) | 22.9-27.1 | 312 | 1.032 ( 0.085) | 1.082 ( 0.300) | 1.131 ( 0.555) | 27.1-30.6 | 312 | 1.004 ( 0.072) | 1.004 ( 0.249) | 1.203 ( 0.498) | 30.6-33.8 | 312 | 0.974 ( 0.074) | 0.925 ( 0.092) | 1.178 ( 0.508) | 33.8-36.9 | 312 | 0.953 ( 0.069) | 0.904 ( 0.113) | 1.145 ( 0.467) | 36.9-39.7 | 312 | 0.934 ( 0.079) | 0.871 ( 0.140) | 1.209 ( 0.555) | 39.7-42.7 | 312 | 0.918 ( 0.070) | 0.835 ( 0.087) | 1.182 ( 0.529) | 42.7-50.7 | 310 | 0.918 ( 0.082) | 0.809 ( 0.065) | 1.153 ( 0.477) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3118 | 0.999 ( 0.104) | 0.992 ( 0.281) | 1.177 ( 0.588) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0017 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708040 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:31:17 2018 PROFFITMAIN - Started at Tue Mar 27 16:31:17 2018 OTKP changes: 3108 2 4 6 OTKP changes: 3108 2 4 6 No constraint UB - matrix: -0.025051 -0.079515 -0.015610 ( 0.000005 0.000005 0.000005 ) 0.072519 -0.029287 0.032925 ( 0.000005 0.000005 0.000005 ) -0.036237 -0.003593 0.076588 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007193 0.000002 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000002 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025051 -0.079515 -0.015610 ( 0.000005 0.000005 0.000005 ) 0.072519 -0.029287 0.032925 ( 0.000005 0.000005 0.000005 ) -0.036237 -0.003593 0.076588 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000000 ) UB fit with 3113 obs out of 3118 (total:3118,skipped:0) (99.84%) unit cell: 8.3594(5) 8.3631(5) 8.3630(4) 90.014(5) 90.027(5) 89.986(5) V = 584.66(6) unit cell: 8.36181(13) 8.36181(13) 8.36181(13) 90.0 90.0 90.0 V = 584.657(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024723 -0.079528 -0.015416 ( 0.000014 0.000011 0.000013 ) 0.072527 -0.028881 0.033051 ( 0.000012 0.000010 0.000012 ) -0.036071 -0.003520 0.076553 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007173 -0.000002 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007171 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3752(12) 8.3759(12) 8.3648(12) 90.016(11) 90.135(11) 89.988(11) V = 586.79(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3580(11) 8.3645(11) 8.3499(11) 90.050(11) 90.081(11) 89.972(11) V = 583.75(14) unit cell: 8.3575(4) 8.3575(4) 8.3575(4) 90.0 90.0 90.0 V = 583.75(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.730) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3580(11) 8.3645(11) 8.3499(11) 90.050(11) 90.081(11) 89.972(11) V = 583.75(14) unit cell: 8.3575(4) 8.3575(4) 8.3575(4) 90.0 90.0 90.0 V = 583.75(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007202 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007216 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024706 -0.079635 -0.015547 ( 0.000013 0.000011 0.000013 ) 0.072649 -0.028917 0.033106 ( 0.000012 0.000010 0.000012 ) -0.036246 -0.003581 0.076671 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3580(11) 8.3645(11) 8.3499(11) 90.050(11) 90.081(11) 89.972(11) V = 583.75(14) unit cell: 8.3575(4) 8.3575(4) 8.3575(4) 90.0 90.0 90.0 V = 583.75(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024856 -0.079563 -0.015645 ( 0.000013 0.000015 0.000011 ) 0.072447 -0.029187 0.032941 ( 0.000016 0.000018 0.000013 ) -0.036281 -0.003656 0.076381 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007196 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3693(14) 8.3618(14) 8.3802(10) 90.033(12) 90.033(12) 89.966(14) V = 586.46(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024994 -0.079536 -0.015503 ( 0.000017 0.000014 0.000012 ) 0.072495 -0.029265 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036257 -0.003619 0.076525 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007195 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000010 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3622(11) 8.3618(14) 8.3677(11) 89.923(12) 90.042(11) 89.981(12) V = 585.09(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007208 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3526(11) 8.3548(14) 8.3600(11) 89.934(12) 90.003(11) 89.965(12) V = 583.40(15) unit cell: 8.3558(3) 8.3558(3) 8.3558(3) 90.0 90.0 90.0 V = 583.40(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.730) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007208 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3526(11) 8.3548(14) 8.3600(11) 89.934(12) 90.003(11) 89.965(12) V = 583.40(15) unit cell: 8.3558(3) 8.3558(3) 8.3558(3) 90.0 90.0 90.0 V = 583.40(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007211 -0.000004 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007208 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079603 -0.015463 ( 0.000016 0.000014 0.000012 ) 0.072573 -0.029296 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036302 -0.003556 0.076620 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3526(11) 8.3548(14) 8.3600(11) 89.934(12) 90.003(11) 89.965(12) V = 583.40(15) unit cell: 8.3558(3) 8.3558(3) 8.3558(3) 90.0 90.0 90.0 V = 583.40(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025028 -0.079531 -0.015724 ( 0.000008 0.000013 0.000012 ) 0.072414 -0.029343 0.032922 ( 0.000008 0.000014 0.000014 ) -0.036206 -0.003658 0.076530 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3702(11) 8.3594(12) 8.3662(11) 90.036(11) 90.054(11) 89.985(11) V = 585.38(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007211 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3634(10) 8.3529(12) 8.3562(11) 89.995(11) 90.025(10) 90.023(11) V = 583.75(13) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.75(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.730) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007211 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3634(10) 8.3529(12) 8.3562(11) 89.995(11) 90.025(10) 90.023(11) V = 583.75(13) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.75(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007193 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007211 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007205 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025079 -0.079587 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072420 -0.029377 0.033011 ( 0.000008 0.000014 0.000013 ) -0.036321 -0.003701 0.076601 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3634(10) 8.3529(12) 8.3562(11) 89.995(11) 90.025(10) 90.023(11) V = 583.75(13) unit cell: 8.3575(3) 8.3575(3) 8.3575(3) 90.0 90.0 90.0 V = 583.75(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025243 -0.079452 -0.015758 ( 0.000011 0.000016 0.000017 ) 0.072368 -0.029418 0.032790 ( 0.000008 0.000011 0.000012 ) -0.036254 -0.003622 0.076603 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007189 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3658(10) 8.3643(14) 8.3642(11) 90.079(12) 89.948(10) 90.064(12) V = 585.27(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007210 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3575(10) 8.3582(14) 8.3535(11) 90.050(12) 89.988(10) 90.063(12) V = 583.52(14) unit cell: 8.3564(3) 8.3564(3) 8.3564(3) 90.0 90.0 90.0 V = 583.52(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.730) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007210 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3575(10) 8.3582(14) 8.3535(11) 90.050(12) 89.988(10) 90.063(12) V = 583.52(14) unit cell: 8.3564(3) 8.3564(3) 8.3564(3) 90.0 90.0 90.0 V = 583.52(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007203 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007210 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079518 -0.015750 ( 0.000011 0.000016 0.000017 ) 0.072489 -0.029414 0.032812 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003663 0.076715 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3575(10) 8.3582(14) 8.3535(11) 90.050(12) 89.988(10) 90.063(12) V = 583.52(14) unit cell: 8.3564(3) 8.3564(3) 8.3564(3) 90.0 90.0 90.0 V = 583.52(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025308 -0.079442 -0.015637 ( 0.000010 0.000008 0.000010 ) 0.072446 -0.029449 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036122 -0.003536 0.076588 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000005 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000005 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007185 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3628(13) 8.3645(9) 8.3676(12) 90.046(10) 90.039(12) 90.038(10) V = 585.32(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3578(13) 8.3594(9) 8.3549(12) 90.069(10) 90.049(12) 90.027(10) V = 583.72(14) unit cell: 8.3574(3) 8.3574(3) 8.3574(3) 90.0 90.0 90.0 V = 583.72(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.730) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3578(13) 8.3594(9) 8.3549(12) 90.069(10) 90.049(12) 90.027(10) V = 583.72(14) unit cell: 8.3574(3) 8.3574(3) 8.3574(3) 90.0 90.0 90.0 V = 583.72(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007202 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007207 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079483 -0.015728 ( 0.000011 0.000008 0.000010 ) 0.072512 -0.029483 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036106 -0.003581 0.076713 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3578(13) 8.3594(9) 8.3549(12) 90.069(10) 90.049(12) 90.027(10) V = 583.72(14) unit cell: 8.3574(3) 8.3574(3) 8.3574(3) 90.0 90.0 90.0 V = 583.72(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb *** 3D integration started - run 7 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" UB fit with 394 obs out of 394 (total:394,skipped:0) (100.00%) UB - matrix: -0.025221 -0.079287 -0.015699 ( 0.000014 0.000011 0.000011 ) 0.072336 -0.029536 0.032900 ( 0.000017 0.000014 0.000014 ) -0.036171 -0.003520 0.076578 ( 0.000016 0.000013 0.000013 ) M - matrix: 0.007177 -0.000009 0.000006 ( 0.000003 0.000002 0.000002 ) -0.000009 0.007171 0.000003 ( 0.000002 0.000002 0.000001 ) 0.000006 0.000003 0.007193 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3726(15) 8.3760(12) 8.3632(14) 90.028(12) 90.047(14) 89.924(13) V = 586.50(17) OTKP changes: 394 1 1 1 No constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007171 -0.000004 0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007174 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000002 0.007183 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000001 ) UB fit with 394 obs out of 394 (total:394,skipped:0) (100.00%) unit cell: 8.3761(15) 8.3741(12) 8.3690(13) 89.983(12) 90.016(14) 89.965(13) V = 587.02(16) unit cell: 8.3731(3) 8.3731(3) 8.3731(3) 90.0 90.0 90.0 V = 587.02(4) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) HKL list info: 669 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007171 -0.000004 0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007174 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000002 0.007183 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000001 ) UB fit with 394 obs out of 394 (total:394,skipped:0) (100.00%) unit cell: 8.3761(15) 8.3741(12) 8.3690(13) 89.983(12) 90.016(14) 89.965(13) V = 587.02(16) unit cell: 8.3731(3) 8.3731(3) 8.3731(3) 90.0 90.0 90.0 V = 587.02(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 394 obs out of 394 (total:394,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 7) ******* No constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007171 -0.000004 0.000002 ( 0.000003 0.000002 0.000002 ) -0.000004 0.007174 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 -0.000002 0.007183 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025231 -0.079297 -0.015709 ( 0.000014 0.000011 0.000011 ) 0.072299 -0.029550 0.032823 ( 0.000017 0.000014 0.000014 ) -0.036155 -0.003631 0.076544 ( 0.000015 0.000012 0.000012 ) M - matrix: 0.007175 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007175 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007175 ( 0.000000 0.000000 0.000001 ) UB fit with 394 obs out of 394 (total:394,skipped:0) (100.00%) unit cell: 8.3761(15) 8.3741(12) 8.3690(13) 89.983(12) 90.016(14) 89.965(13) V = 587.02(16) unit cell: 8.3731(3) 8.3731(3) 8.3731(3) 90.0 90.0 90.0 V = 587.02(4) *** End best per run unit cell (run 7) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=91, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=67, end=91, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_7_67.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_7_67.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_7_67.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025054 -0.079470 -0.015589 ( 0.000006 0.000006 0.000006 ) 0.072514 -0.029300 0.032888 ( 0.000006 0.000006 0.000006 ) -0.036252 -0.003631 0.076592 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000002 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007187 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000003 0.007191 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025054 -0.079470 -0.015589 ( 0.000006 0.000006 0.000006 ) 0.072514 -0.029300 0.032888 ( 0.000006 0.000006 0.000006 ) -0.036252 -0.003631 0.076592 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) UB fit with 3113 obs out of 3118 (total:3118,skipped:0) (99.84%) unit cell: 8.3591(6) 8.3666(6) 8.3644(4) 89.978(5) 89.990(5) 89.984(5) V = 584.98(6) unit cell: 8.36337(17) 8.36337(17) 8.36337(17) 90.0 90.0 90.0 V = 584.98(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 76 reflections under beam stop or inside a detector rejection region 24 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof 4220 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:31:27 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.730) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.730) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.730) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.730) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.730) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) PROFFIT INFO: signal sum: min=119.0000 max=23193580.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3188061.4882 PROFFIT INFO: background sum: min=619.0000 max=26597.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=12423.0000 PROFFIT INFO: num of signal pixels: min=50 max=545 PROFFIT INFO: Inet: min=293.3857 max=5100898.5000 PROFFIT INFO: sig(Inet): min=120.2458 max=47812.4453 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 57 223 471 865 979 1792 2847 3886 4220 Percent 0.0 0.0 1.4 5.3 11.2 20.5 23.2 42.5 67.5 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4220 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4220 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100899- 1085882 422 1813592.57 121.55 100.00 1084838- 590774 422 811948.65 100.49 100.00 589229- 251034 422 391053.58 93.33 100.00 250565- 163253 422 195024.31 70.14 100.00 163180- 114566 422 137643.27 49.18 100.00 114431- 87202 422 100016.61 34.95 100.00 87190- 60752 422 74931.01 28.01 100.00 60600- 5128 422 32717.47 17.99 100.00 5106- 2791 422 3679.45 5.16 95.26 2785- 293 422 1980.35 3.60 51.90 ------------------------------------------------------------------------------------ 5100899- 293 4220 356258.73 52.44 94.72 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 731693.87 91.22 100.00 1.41- 1.12 422 576906.59 64.29 99.29 1.12- 0.96 422 498860.56 69.69 96.92 0.96- 0.87 422 329739.98 58.13 93.84 0.87- 0.81 422 434347.06 67.59 99.29 0.81- 0.73 422 236276.41 40.40 95.97 0.73- 0.71 422 169071.64 33.64 87.91 0.71- 0.65 422 295415.49 45.74 93.13 0.65- 0.62 422 148180.79 27.06 87.68 0.62- 0.58 422 142094.88 26.64 93.13 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 356258.73 52.44 94.72 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:31:27 2018 Sorting 4220 observations 119 unique observations with > 7.00 F2/sig(F2) 4220 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 Total number of frames 718 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4220 observations in 7 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 Total number of frames 107 3381 observations > 7.00 F2/sig(F2) 3381 observations in 7 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 Total number of frames 107 Removing 'redundancy=1' reflections Average redundancy: 26.0 (Out of 3381 removed 4 = 3377, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3377 observations in 7 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 Total number of frames 107 130 unique data precomputed (should be 130) 130 unique data with 3377 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.0 (Out of 3377 removed 0 = 3377, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3377 observations RMS deviation of equivalent data = 0.26588 Rint = 0.20341 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19925, wR= 0.28235 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15457, wR= 0.20310, Acormin=0.565, Acormax=1.338, Acor_av=0.996 F test: Probability=1.000, F= 1.659 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13110, wR= 0.17039, Acormin=0.539, Acormax=1.434, Acor_av=0.943 F test: Probability=1.000, F= 1.389 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13137, wR= 0.17548, Acormin=0.579, Acormax=1.577, Acor_av=0.974 F test: Probability=0.000, F= 0.994 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10386, wR= 0.13882, Acormin=0.500, Acormax=1.587, Acor_av=0.933 F test: Probability=1.000, F= 1.589 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09213, wR= 0.12525, Acormin=0.469, Acormax=1.632, Acor_av=0.944 F test: Probability=1.000, F= 1.268 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11861, wR= 0.16317, Acormin=0.607, Acormax=1.639, Acor_av=0.981 F test: Probability=0.000, F= 0.603 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09412, wR= 0.12906, Acormin=0.497, Acormax=1.671, Acor_av=0.938 F test: Probability=0.000, F= 0.956 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08499, wR= 0.11815, Acormin=0.476, Acormax=1.671, Acor_av=0.946 F test: Probability=1.000, F= 1.170 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08154, wR= 0.11193, Acormin=0.326, Acormax=1.547, Acor_av=0.883 F test: Probability=0.988, F= 1.083 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11878, wR= 0.15437, Acormin=0.421, Acormax=1.441, Acor_av=0.831 F test: Probability=0.000, F= 0.472 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09358, wR= 0.12645, Acormin=0.495, Acormax=1.628, Acor_av=0.922 F test: Probability=0.000, F= 0.760 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09427, wR= 0.12380, Acormin=0.076, Acormax=0.337, Acor_av=0.181 F test: Probability=0.000, F= 0.747 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08512, wR= 0.11351, Acormin=0.073, Acormax=0.376, Acor_av=0.202 F test: Probability=0.000, F= 0.913 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07784, wR= 0.10492, Acormin=0.075, Acormax=0.402, Acor_av=0.213 F test: Probability=0.990, F= 1.086 Final absorption model (ne=6, no=5): Rint= 0.08154, Acormin=0.326, Acormax=1.547, Acor_av=0.883 Combined refinement in use Rint: 0.20352 There are 107 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 154 pars with 11935 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26588 Using Levenberg-Marquardt: 0.00010 New wR= 0.06898 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20341 with corrections 0.05372 Rint for all data: 0.20352 with corrections 0.05395 0 observations identified as outliers and rejected Cycle 2 wR= 0.06898 Using Levenberg-Marquardt: 0.00001 New wR= 0.06402 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20341 with corrections 0.04923 Rint for all data: 0.20352 with corrections 0.04946 0 observations identified as outliers and rejected Cycle 3 wR= 0.06402 Using Levenberg-Marquardt: 0.00000 New wR= 0.06246 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20341 with corrections 0.04821 Rint for all data: 0.20352 with corrections 0.04844 1 observations identified as outliers and rejected Cycle 4 wR= 0.06241 Using Levenberg-Marquardt: 0.00000 New wR= 0.06143 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20372 with corrections 0.04745 Rint for all data: 0.20352 with corrections 0.04784 1 observations identified as outliers and rejected Cycle 5 wR= 0.06145 Using Levenberg-Marquardt: 0.00000 New wR= 0.06088 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20259 with corrections 0.04703 Rint for all data: 0.20352 with corrections 0.04747 0 observations identified as outliers and rejected Final wR= 0.06088 Final frame scales: Min= 0.7317 Max= 1.3049 Final absorption correction factors: Amin= 0.4804 Amax= 1.4759 PROFFIT INFO: Inet (after scale3 abspack): min=627.6303 max=4375520.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=134.2506 max=53879.2344 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/7 frame:1/109 4220 reflections read from tmp file 923 reflections are rejected (923 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 2 6 3 3 2 2 3 132 Initial Chi^2= 0.41142 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.86782 Current error model SIG(F2)^2 = 125.58*I_RAW + 0.00*I_BACK+(0.02319*)^2 Cycle 2, Chi^2= 1.00016 Current error model SIG(F2)^2 = 111.88*I_RAW + 0.00*I_BACK+(0.02092*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 111.61*I_RAW + 0.00*I_BACK+(0.02099*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 111.61*I_RAW + 0.00*I_BACK+(0.02099*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4375520- 1037285 422 1684161.22 44.39 100.00 1035850- 571964 422 770351.08 37.33 100.00 571643- 241105 422 378775.85 35.96 100.00 240505- 145829 422 181107.59 31.36 100.00 145717- 117112 422 131700.14 25.41 100.00 116928- 82615 422 95735.38 19.47 100.00 82441- 63958 422 73404.55 16.67 100.00 63904- 4609 422 35353.84 11.65 99.76 4597- 2588 422 3409.92 4.60 95.97 2586- 628 422 2005.41 3.78 72.75 ------------------------------------------------------------------------------------ 4375520- 628 4220 335600.50 23.06 96.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 719811.25 36.07 100.00 1.41- 1.12 422 551932.42 28.54 99.53 1.12- 0.96 422 452507.86 27.51 97.87 0.96- 0.87 422 306175.78 23.71 96.68 0.87- 0.81 422 407098.82 27.22 99.76 0.81- 0.73 422 215108.07 18.83 97.63 0.73- 0.71 422 160629.79 17.43 91.23 0.71- 0.65 422 274439.57 21.90 96.92 0.65- 0.62 422 138280.02 14.66 92.89 0.62- 0.58 422 130021.43 14.74 95.97 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 335600.50 23.06 96.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 719811.25 36.07 100.00 4.82- 1.12 844 635871.83 32.30 99.76 4.82- 0.96 1266 574750.51 30.71 99.13 4.82- 0.87 1688 507606.83 28.96 98.52 4.82- 0.81 2110 487505.22 28.61 98.77 4.82- 0.73 2532 442105.70 26.98 98.58 4.82- 0.71 2954 401894.85 25.62 97.53 4.82- 0.65 3376 385962.94 25.15 97.45 4.82- 0.62 3798 358442.62 23.99 96.95 4.82- 0.58 4220 335600.50 23.06 96.85 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 335600.50 23.06 96.85 Scale applied to data: s=0.228544 (maximum obs:4375520.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.047; Rsigma 0.028: data 4220 -> merged 157 With outlier rejection... Rint 0.047; Rsigma 0.028: data 4207 -> merged 157 Rejected total: 13, method kkm 11, method Blessing 2 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585553, 4.828596 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.48 14 14 25.07 100.00 351 1.41 - 1.12 14 14 34.57 100.00 484 1.12 - 0.97 14 14 34.71 100.00 486 0.96 - 0.84 14 14 36.79 100.00 515 0.84 - 0.78 14 14 28.07 100.00 393 0.78 - 0.73 14 14 29.79 100.00 417 0.73 - 0.69 14 14 27.50 100.00 385 0.69 - 0.66 14 14 23.50 100.00 329 0.65 - 0.63 14 14 24.79 100.00 347 0.63 - 0.60 14 14 21.64 100.00 303 --------------------------------------------------------------- 8.38 - 0.60 140 140 28.64 100.00 4010 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:31:28 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.359080 8.366629 8.364414 89.9776 89.9900 89.9845 4207 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2147 0 2818 2820 4207 N (int>3sigma) = 0 0 0 0 2147 0 2729 2730 4074 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 77.3 79.2 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 23.1 23.3 23.1 Lattice type: F chosen Volume: 584.98 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.913 5.913 119.96 90.04 119.98 Niggli form: a.a = 34.953 b.b = 34.959 c.c = 34.966 b.c = -17.460 a.c = -0.022 a.b = -17.468 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.030 CUBIC F-lattice R(int) = 0.047 [ 4050] Vol = 585.0 Cell: 8.359 8.367 8.364 90.02 89.99 90.02 Volume: 584.98 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.029 RHOMBOHEDRAL R-lattice R(int) = 0.052 [ 3766] Vol = 438.7 Cell: 5.913 5.912 14.490 89.97 90.05 119.98 Volume: 438.74 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.029 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1194] Vol = 438.7 Trigonal Cell: 5.913 5.912 14.490 89.97 90.05 119.98 Volume: 438.74 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.033 TETRAGONAL I-lattice R(int) = 0.046 [ 3801] Vol = 292.5 Cell: 5.914 5.916 8.359 89.98 90.00 90.02 Volume: 292.49 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.027 TETRAGONAL I-lattice R(int) = 0.046 [ 3801] Vol = 292.5 Cell: 5.914 5.916 8.359 89.98 90.00 90.02 Volume: 292.49 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3747] Vol = 292.5 Cell: 5.914 8.359 5.916 89.98 89.98 90.00 Volume: 292.49 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.008 MONOCLINIC I-lattice R(int) = 0.045 [ 3394] Vol = 292.5 Cell: 8.359 5.914 5.916 90.02 90.02 90.00 Volume: 292.49 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.024 MONOCLINIC I-lattice R(int) = 0.044 [ 3391] Vol = 292.5 Cell: 5.913 5.912 8.367 90.00 90.03 89.96 Volume: 292.49 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC C-lattice R(int) = 0.044 [ 3405] Vol = 292.5 Cell: 8.359 8.367 5.912 90.00 134.98 90.02 Volume: 292.49 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2718] Vol = 146.2 Cell: 5.912 5.913 5.913 119.96 90.04 119.98 Volume: 146.25 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2147 0 2816 2836 4207 N (int>3sigma) = 0 0 0 0 2147 0 2723 2744 4074 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 76.7 78.2 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 23.1 23.2 23.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.166 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 322 943 N I>3s 45 45 306 943 1.0 1.0 0.7 36.1 9.0 9.0 5.5 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3748 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3787 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359080 8.366629 8.364414 90.0224 89.9900 90.0155 ZERR 3.00 0.000574 0.000558 0.000452 0.0049 0.0050 0.0055 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3749209- 705309 686 686 26 26.4 1360597.34 42.10 0.042 0.056 701597- 211884 653 648 26 24.9 425501.08 36.04 0.059 0.072 208177- 91954 977 977 26 37.6 140453.96 26.14 0.046 0.059 89471- 63004 689 688 26 26.5 77378.34 16.94 0.068 0.088 60925- 3318 535 531 26 20.4 23371.44 8.89 0.084 0.114 3226- 1671 680 677 27 25.1 2520.98 4.28 0.203 0.270 ------------------------------------------------------------------------------------------- 3749209- 1671 4220 4207 157 26.8 336028.34 23.07 0.047 0.062 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 794 790 26 30.4 584809.80 31.62 0.046 0.062 0.023 1.12-0.88 931 929 26 35.7 431023.02 26.77 0.037 0.049 0.026 0.85-0.75 778 778 26 29.9 311423.86 22.55 0.046 0.058 0.029 0.74-0.68 684 684 26 26.3 246659.83 20.34 0.058 0.071 0.033 0.67-0.63 647 647 26 24.9 139391.58 15.89 0.070 0.088 0.042 0.62-0.59 386 379 27 14.0 132088.83 14.43 0.072 0.068 0.043 ------------------------------------------------------------------------------------------------------ inf-0.59 4220 4207 157 26.8 336028.34 23.07 0.047 0.062 0.028 inf-0.60 4016 4008 139 28.8 348174.36 23.56 0.047 0.062 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 790 26 26 100.0 30.4 584809.80 188.69 0.046 0.005 1.12-0.88 929 26 26 100.0 35.7 431023.02 162.69 0.037 0.005 0.85-0.75 778 26 26 100.0 29.9 311423.86 130.23 0.046 0.005 0.74-0.68 684 26 26 100.0 26.3 246659.83 106.71 0.058 0.007 0.67-0.63 647 26 26 100.0 24.9 139391.58 78.62 0.070 0.009 0.62-0.59 379 27 27 100.0 14.0 132088.83 62.45 0.072 0.016 -------------------------------------------------------------------------------------------- inf-0.59 4207 157 157 100.0 26.8 336028.34 130.51 0.047 0.006 inf-0.60 4008 139 139 100.0 28.8 348174.36 134.49 0.047 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025054 -0.079470 -0.015589 ( 0.000005 0.000006 0.000006 ) 0.072514 -0.029299 0.032888 ( 0.000006 0.000006 0.000006 ) -0.036252 -0.003631 0.076592 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000002 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007187 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000003 0.007191 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025054 -0.079470 -0.015589 ( 0.000005 0.000006 0.000006 ) 0.072514 -0.029299 0.032888 ( 0.000006 0.000006 0.000006 ) -0.036252 -0.003631 0.076592 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007191 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007191 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007191 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3591(6) 8.3667(6) 8.3644(4) 89.977(5) 89.990(5) 89.984(5) V = 584.99(6) unit cell: 8.36338(17) 8.36338(17) 8.36338(17) 90.0 90.0 90.0 V = 584.99(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.730) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.730) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.730) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.730) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.730) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) PROFFIT INFO: signal sum: min=119.0000 max=23193580.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3188061.4882 PROFFIT INFO: background sum: min=619.0000 max=26597.0000 PROFFIT INFO: background sum sig2: min=554.0000 max=12423.0000 PROFFIT INFO: num of signal pixels: min=50 max=545 PROFFIT INFO: Inet: min=293.3857 max=5100898.5000 PROFFIT INFO: sig(Inet): min=120.2458 max=47812.4453 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.60 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 114 446 942 1730 1958 3584 5694 7772 8440 Percent 0.0 0.0 1.4 5.3 11.2 20.5 23.2 42.5 67.5 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4220 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4220 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100899- 1085882 422 1813592.57 121.55 100.00 1084838- 590774 422 811948.65 100.49 100.00 589229- 251034 422 391053.58 93.33 100.00 250565- 163253 422 195024.31 70.14 100.00 163180- 114566 422 137643.27 49.18 100.00 114431- 87202 422 100016.61 34.95 100.00 87190- 60752 422 74931.01 28.01 100.00 60600- 5128 422 32717.47 17.99 100.00 5106- 2791 422 3679.45 5.16 95.26 2785- 293 422 1980.35 3.60 51.90 ------------------------------------------------------------------------------------ 5100899- 293 4220 356258.73 52.44 94.72 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 731693.87 91.22 100.00 1.41- 1.12 422 576906.59 64.29 99.29 1.12- 0.96 422 498860.56 69.69 96.92 0.96- 0.87 422 329739.98 58.13 93.84 0.87- 0.81 422 434347.06 67.59 99.29 0.81- 0.73 422 236276.41 40.40 95.97 0.73- 0.71 422 169071.64 33.64 87.91 0.71- 0.65 422 295415.49 45.74 93.13 0.65- 0.62 422 148180.79 27.06 87.68 0.62- 0.58 422 142094.88 26.64 93.13 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 356258.73 52.44 94.72 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:31:28 2018 Sorting 4220 observations 85 unique observations with > 7.00 F2/sig(F2) 4220 observations in 7 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 Total number of frames 718 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4220 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 Total number of frames 81 3381 observations > 7.00 F2/sig(F2) 3381 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 36.3 (Out of 3381 removed 4 = 3377, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3377 observations in 7 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 Total number of frames 81 93 unique data precomputed (should be 93) 93 unique data with 3377 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 36.3 (Out of 3377 removed 0 = 3377, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3377 observations RMS deviation of equivalent data = 0.26653 Rint = 0.20371 6 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19936, wR= 0.28290 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15496, wR= 0.20364, Acormin=0.564, Acormax=1.338, Acor_av=0.996 F test: Probability=1.000, F= 1.653 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13139, wR= 0.17096, Acormin=0.539, Acormax=1.435, Acor_av=0.944 F test: Probability=1.000, F= 1.390 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13157, wR= 0.17588, Acormin=0.580, Acormax=1.579, Acor_av=0.974 F test: Probability=0.000, F= 0.996 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10396, wR= 0.13927, Acormin=0.499, Acormax=1.590, Acor_av=0.933 F test: Probability=1.000, F= 1.593 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09227, wR= 0.12585, Acormin=0.466, Acormax=1.634, Acor_av=0.944 F test: Probability=1.000, F= 1.267 Trying model 6 (ne=6, no=0)... Results: Rint= 0.11855, wR= 0.16360, Acormin=0.606, Acormax=1.646, Acor_av=0.983 F test: Probability=0.000, F= 0.605 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09425, wR= 0.12950, Acormin=0.498, Acormax=1.667, Acor_av=0.939 F test: Probability=0.000, F= 0.957 Trying model 8 (ne=6, no=3)... Results: Rint= 0.08515, wR= 0.11869, Acormin=0.478, Acormax=1.680, Acor_av=0.947 F test: Probability=1.000, F= 1.169 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08189, wR= 0.11249, Acormin=0.327, Acormax=1.550, Acor_av=0.885 F test: Probability=0.983, F= 1.078 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11888, wR= 0.15488, Acormin=0.426, Acormax=1.443, Acor_av=0.832 F test: Probability=0.000, F= 0.475 Trying model 11 (ne=8, no=1)... Results: Rint= 0.09356, wR= 0.12689, Acormin=0.498, Acormax=1.634, Acor_av=0.923 F test: Probability=0.000, F= 0.766 Trying model 12 (ne=8, no=3)... Results: Rint= 0.09457, wR= 0.12477, Acormin=0.075, Acormax=0.334, Acor_av=0.179 F test: Probability=0.000, F= 0.748 Trying model 13 (ne=8, no=5)... Results: Rint= 0.08563, wR= 0.11466, Acormin=0.073, Acormax=0.371, Acor_av=0.199 F test: Probability=0.000, F= 0.910 Trying model 14 (ne=8, no=7)... Results: Rint= 0.07821, wR= 0.10574, Acormin=0.073, Acormax=0.396, Acor_av=0.209 F test: Probability=0.990, F= 1.085 Final absorption model (ne=6, no=5): Rint= 0.08189, Acormin=0.327, Acormax=1.550, Acor_av=0.885 Combined refinement in use Rint: 0.20381 There are 81 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26653 Using Levenberg-Marquardt: 0.00010 New wR= 0.07184 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20371 with corrections 0.05590 Rint for all data: 0.20381 with corrections 0.05613 1 observations identified as outliers and rejected Cycle 2 wR= 0.07181 Using Levenberg-Marquardt: 0.00001 New wR= 0.06679 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20348 with corrections 0.05130 Rint for all data: 0.20381 with corrections 0.05156 0 observations identified as outliers and rejected Cycle 3 wR= 0.06679 Using Levenberg-Marquardt: 0.00000 New wR= 0.06500 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20348 with corrections 0.05005 Rint for all data: 0.20381 with corrections 0.05031 0 observations identified as outliers and rejected Cycle 4 wR= 0.06500 Using Levenberg-Marquardt: 0.00000 New wR= 0.06388 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20348 with corrections 0.04931 Rint for all data: 0.20381 with corrections 0.04957 0 observations identified as outliers and rejected Cycle 5 wR= 0.06388 Using Levenberg-Marquardt: 0.00000 New wR= 0.06310 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20348 with corrections 0.04880 Rint for all data: 0.20381 with corrections 0.04906 1 observations identified as outliers and rejected Final wR= 0.06310 Final frame scales: Min= 0.7854 Max= 1.2817 Final absorption correction factors: Amin= 0.4716 Amax= 1.4301 PROFFIT INFO: Inet (after scale3 abspack): min=642.9941 max=4472603.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=131.5300 max=52687.5078 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/7 frame:1/109 4220 reflections read from tmp file 936 reflections are rejected (936 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 2 3 1 3 1 2 2 95 Initial Chi^2= 0.40536 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.87487 Current error model SIG(F2)^2 = 133.60*I_RAW + 0.00*I_BACK+(0.02216*)^2 Cycle 2, Chi^2= 0.99999 Current error model SIG(F2)^2 = 114.37*I_RAW + 0.00*I_BACK+(0.02124*)^2 Cycle 3, Chi^2= 1.00001 Current error model SIG(F2)^2 = 114.69*I_RAW + 0.00*I_BACK+(0.02117*)^2 Final Chi^2= 1.00001 Final error model SIG(F2)^2 = 114.69*I_RAW + 0.00*I_BACK+(0.02117*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4472603- 1041899 422 1678661.19 43.98 100.00 1036571- 574314 422 770573.66 36.96 100.00 574135- 239278 422 378438.16 35.56 100.00 239243- 145620 422 180790.53 31.03 100.00 145450- 116619 422 131856.26 25.09 100.00 116568- 82832 422 95877.01 19.21 100.00 82816- 63343 422 73455.89 16.53 100.00 63341- 4597 422 35334.35 11.46 99.76 4596- 2596 422 3409.48 4.52 95.02 2586- 643 422 2003.50 3.74 71.56 ------------------------------------------------------------------------------------ 4472603- 643 4220 335040.00 22.81 96.64 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 715871.53 35.70 100.00 1.41- 1.12 422 550396.97 28.25 99.53 1.12- 0.96 422 450976.17 27.22 97.87 0.96- 0.87 422 306462.04 23.45 96.45 0.87- 0.81 422 406818.05 26.93 99.76 0.81- 0.73 422 215018.80 18.62 97.16 0.73- 0.71 422 160883.99 17.22 90.76 0.71- 0.65 422 275051.78 21.65 96.92 0.65- 0.62 422 138580.41 14.49 92.18 0.62- 0.58 422 130340.29 14.56 95.73 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 335040.00 22.81 96.64 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 422 715871.53 35.70 100.00 4.82- 1.12 844 633134.25 31.98 99.76 4.82- 0.96 1266 572414.89 30.39 99.13 4.82- 0.87 1688 505926.68 28.66 98.46 4.82- 0.81 2110 486104.95 28.31 98.72 4.82- 0.73 2532 440923.93 26.69 98.46 4.82- 0.71 2954 400918.22 25.34 97.36 4.82- 0.65 3376 385184.92 24.88 97.30 4.82- 0.62 3798 357784.41 23.72 96.74 4.82- 0.58 4220 335040.00 22.81 96.64 ------------------------------------------------------------------------------------ 4.82- 0.58 4220 335040.00 22.81 96.64 Scale applied to data: s=0.223583 (maximum obs:4472603.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.049; Rsigma 0.028: data 4220 -> merged 110 With outlier rejection... Rint 0.048; Rsigma 0.028: data 4205 -> merged 110 Rejected total: 15, method kkm 11, method Blessing 4 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585554, 4.828602 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.38 - 1.71 10 10 26.60 100.00 266 1.61 - 1.21 10 10 39.00 100.00 390 1.17 - 1.01 10 10 50.20 100.00 502 0.99 - 0.89 10 10 48.20 100.00 482 0.88 - 0.81 10 10 46.50 100.00 465 0.81 - 0.74 10 10 40.60 100.00 406 0.73 - 0.71 10 10 44.60 100.00 446 0.70 - 0.66 10 10 36.90 100.00 369 0.66 - 0.64 10 10 34.80 100.00 348 0.63 - 0.60 10 10 33.10 100.00 331 --------------------------------------------------------------- 8.38 - 0.60 100 100 40.05 100.00 4005 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:31:28 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.359080 8.366629 8.364414 89.9776 89.9900 89.9845 4207 Reflections read from file xs1714a.hkl; mean (I/sigma) = 23.07 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2147 0 2818 2820 4207 N (int>3sigma) = 0 0 0 0 2147 0 2729 2730 4074 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 77.3 79.2 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 23.1 23.3 23.1 Lattice type: F chosen Volume: 584.98 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.913 5.913 119.96 90.04 119.98 Niggli form: a.a = 34.953 b.b = 34.959 c.c = 34.966 b.c = -17.460 a.c = -0.022 a.b = -17.468 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.030 CUBIC F-lattice R(int) = 0.047 [ 4050] Vol = 585.0 Cell: 8.359 8.367 8.364 90.02 89.99 90.02 Volume: 584.98 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.029 RHOMBOHEDRAL R-lattice R(int) = 0.052 [ 3766] Vol = 438.7 Cell: 5.913 5.912 14.490 89.97 90.05 119.98 Volume: 438.74 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.029 RHOMBOHEDRAL R-lattice R(int) = 0.044 [ 1194] Vol = 438.7 Trigonal Cell: 5.913 5.912 14.490 89.97 90.05 119.98 Volume: 438.74 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.033 TETRAGONAL I-lattice R(int) = 0.046 [ 3801] Vol = 292.5 Cell: 5.914 5.916 8.359 89.98 90.00 90.02 Volume: 292.49 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.027 TETRAGONAL I-lattice R(int) = 0.046 [ 3801] Vol = 292.5 Cell: 5.914 5.916 8.359 89.98 90.00 90.02 Volume: 292.49 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.016 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 3747] Vol = 292.5 Cell: 5.914 8.359 5.916 89.98 89.98 90.00 Volume: 292.49 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.008 MONOCLINIC I-lattice R(int) = 0.045 [ 3394] Vol = 292.5 Cell: 8.359 5.914 5.916 90.02 90.02 90.00 Volume: 292.49 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.024 MONOCLINIC I-lattice R(int) = 0.044 [ 3391] Vol = 292.5 Cell: 5.913 5.912 8.367 90.00 90.03 89.96 Volume: 292.49 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC C-lattice R(int) = 0.044 [ 3405] Vol = 292.5 Cell: 8.359 8.367 5.912 90.00 134.98 90.02 Volume: 292.49 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.040 [ 2718] Vol = 146.2 Cell: 5.912 5.913 5.913 119.96 90.04 119.98 Volume: 146.25 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2147 0 2816 2836 4207 N (int>3sigma) = 0 0 0 0 2147 0 2723 2744 4074 Mean intensity = 0.0 0.0 0.0 0.0 30.4 0.0 76.7 78.2 76.8 Mean int/sigma = 0.0 0.0 0.0 0.0 23.9 0.0 23.1 23.2 23.1 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.166 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 45 45 322 943 N I>3s 45 45 306 943 1.0 1.0 0.7 36.1 9.0 9.0 5.5 26.6 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.047 3748 Fd-3m 1 1 227 C N N N N 37 2284 0.047 3787 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.359080 8.366629 8.364414 90.0224 89.9900 90.0155 ZERR 3.00 0.000574 0.000558 0.000452 0.0049 0.0050 0.0055 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3717117- 489169 937 935 27 34.6 1152540.81 39.58 0.046 0.058 470028- 112812 1245 1241 27 46.0 200663.60 30.02 0.052 0.065 100244- 33337 1040 1038 27 38.4 74245.52 16.52 0.069 0.087 9808- 1738 998 991 29 34.2 3288.96 4.52 0.171 0.221 ------------------------------------------------------------------------------------------- 3717117- 1738 4220 4205 110 38.2 334595.81 22.80 0.048 0.061 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1075 1068 27 39.6 596731.42 32.05 0.043 0.057 0.024 1.01-0.78 1258 1255 27 46.5 316625.49 22.48 0.042 0.052 0.028 0.78-0.65 1116 1115 28 39.8 233046.74 19.30 0.058 0.070 0.034 0.65-0.59 771 767 28 27.4 146615.55 15.54 0.075 0.083 0.042 ------------------------------------------------------------------------------------------------------ inf-0.59 4220 4205 110 38.2 334595.81 22.80 0.048 0.061 0.028 inf-0.60 4016 4003 99 40.4 346553.45 23.29 0.048 0.061 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1068 27 27 100.0 39.6 596731.42 225.80 0.043 0.005 1.01-0.78 1255 27 27 100.0 46.5 316625.49 162.63 0.042 0.004 0.78-0.65 1115 28 28 100.0 39.8 233046.74 129.37 0.058 0.006 0.65-0.59 767 28 28 100.0 27.4 146615.55 93.44 0.075 0.011 -------------------------------------------------------------------------------------------- inf-0.59 4205 110 110 100.0 38.2 334595.81 157.23 0.048 0.006 inf-0.60 4003 99 99 100.0 40.4 346553.45 161.58 0.048 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:37:34 2018) ID: 2932; threads 39; handles 878; mem 518920.00 (1237720.00)kB; time: 1w 5d 1h 43m 5s MEMORY INFO: Memory PF:0.0, Ph:234.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.8,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:1.0, Ph:234.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.5,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:37:34 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) 8.37024 ( 0.00058 ) 8.37691 ( 0.00056 ) 8.37554 ( 0.00045 ) 90.02113 ( 0.00491 ) 90.03240 ( 0.00502 ) 90.03043 ( 0.00548 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:37:35 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000006 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000002 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007187 -0.000003 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000003 0.007191 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(6) 8.3755(4) 90.021(5) 90.032(5) 90.030(5) V = 587.27(6) unit cell: 8.36338(17) 8.36338(17) 8.36338(17) 90.0 90.0 90.0 V = 584.99(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 39 | 1.034 ( 0.140) | 1.212 ( 0.488) | 1.144 ( 0.710) | 1.41- 1.17 | 39 | 1.017 ( 0.109) | 1.175 ( 0.516) | 1.084 ( 0.530) | 1.17- 0.99 | 39 | 1.025 ( 0.094) | 1.047 ( 0.109) | 0.944 ( 0.361) | 0.99- 0.89 | 39 | 1.018 ( 0.096) | 1.012 ( 0.121) | 1.026 ( 0.379) | 0.89- 0.82 | 39 | 1.019 ( 0.086) | 1.008 ( 0.096) | 1.145 ( 0.483) | 0.82- 0.75 | 39 | 1.007 ( 0.087) | 0.964 ( 0.126) | 1.064 ( 0.402) | 0.75- 0.71 | 39 | 0.968 ( 0.066) | 0.899 ( 0.082) | 1.221 ( 0.547) | 0.71- 0.67 | 39 | 0.965 ( 0.044) | 0.877 ( 0.053) | 1.246 ( 0.535) | 0.67- 0.63 | 39 | 0.948 ( 0.039) | 0.830 ( 0.043) | 1.280 ( 0.452) | 0.63- 0.59 | 43 | 0.909 ( 0.040) | 0.782 ( 0.038) | 1.129 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 394 | 0.990 ( 0.094) | 0.978 ( 0.273) | 1.128 ( 0.501) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 8 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb PROFFITPEAK info: 299 peaks in the peak location table UB fit with 138 obs out of 155 (total:155,skipped:0) (89.03%) UB - matrix: -0.025330 -0.079324 -0.015605 ( 0.000065 0.000023 0.000115 ) 0.072453 -0.029464 0.032872 ( 0.000094 0.000033 0.000167 ) -0.036203 -0.003701 0.076638 ( 0.000089 0.000031 0.000158 ) M - matrix: 0.007202 0.000009 0.000002 ( 0.000015 0.000006 0.000016 ) 0.000009 0.007174 -0.000014 ( 0.000006 0.000004 0.000011 ) 0.000002 -0.000014 0.007197 ( 0.000016 0.000011 0.000027 ) unit cell: 8.358(11) 8.374(4) 8.361(14) 89.89(8) 90.02(12) 90.07(7) V = 585(1) UB fit with 138 obs out of 155 (total:155,skipped:0) (89.03%) UB - matrix: -0.025330 -0.079324 -0.015605 ( 0.000065 0.000023 0.000115 ) 0.072453 -0.029464 0.032872 ( 0.000094 0.000033 0.000167 ) -0.036203 -0.003701 0.076638 ( 0.000089 0.000031 0.000158 ) M - matrix: 0.007202 0.000009 0.000002 ( 0.000015 0.000006 0.000016 ) 0.000009 0.007174 -0.000014 ( 0.000006 0.000004 0.000011 ) 0.000002 -0.000014 0.007197 ( 0.000016 0.000011 0.000027 ) unit cell: 8.358(11) 8.374(4) 8.361(14) 89.89(8) 90.02(12) 90.07(7) V = 585(1) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 UB - matrix: -0.025366 -0.079286 -0.015695 ( 0.000064 0.000022 0.000112 ) 0.072463 -0.029552 0.033061 ( 0.000096 0.000033 0.000168 ) -0.036302 -0.003613 0.076546 ( 0.000090 0.000032 0.000159 ) M - matrix: 0.007212 0.000001 0.000015 ( 0.000016 0.000006 0.000016 ) 0.000001 0.007173 -0.000009 ( 0.000006 0.000004 0.000011 ) 0.000015 -0.000009 0.007199 ( 0.000016 0.000011 0.000027 ) UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) unit cell: 8.352(11) 8.375(4) 8.360(14) 89.93(8) 90.12(12) 90.01(7) V = 585(1) UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) UB - matrix: -0.025366 -0.079286 -0.015695 ( 0.000064 0.000022 0.000112 ) 0.072463 -0.029552 0.033061 ( 0.000096 0.000033 0.000168 ) -0.036302 -0.003613 0.076546 ( 0.000090 0.000032 0.000159 ) M - matrix: 0.007212 0.000001 0.000015 ( 0.000016 0.000006 0.000016 ) 0.000001 0.007173 -0.000009 ( 0.000006 0.000004 0.000011 ) 0.000015 -0.000009 0.007199 ( 0.000016 0.000011 0.000027 ) unit cell: 8.352(11) 8.375(4) 8.360(14) 89.93(8) 90.12(12) 90.01(7) V = 585(1) OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 OTKP changes: 25 1 1 1 155 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Run 8 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 273 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025366 -0.079286 -0.015695 ( 0.000064 0.000022 0.000112 ) 0.072463 -0.029552 0.033061 ( 0.000096 0.000033 0.000168 ) -0.036302 -0.003613 0.076546 ( 0.000090 0.000032 0.000159 ) M - matrix: 0.007212 0.000001 0.000015 ( 0.000016 0.000006 0.000016 ) 0.000001 0.007173 -0.000009 ( 0.000006 0.000004 0.000011 ) 0.000015 -0.000009 0.007199 ( 0.000016 0.000011 0.000027 ) UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) unit cell: 8.352(11) 8.375(4) 8.360(14) 89.93(8) 90.12(12) 90.01(7) V = 585(1) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 139 obs out of 155 (total:155,skipped:0) (89.68%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb 2 of 102 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 100 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 100 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 1.41 | 10 | 1.058 ( 0.158) | 1.248 ( 0.686) | 0.911 ( 0.306) | 1.41- 1.17 | 10 | 1.090 ( 0.080) | 1.120 ( 0.063) | 0.826 ( 0.175) | 1.15- 1.01 | 10 | 1.034 ( 0.087) | 1.013 ( 0.127) | 1.211 ( 0.555) | 0.98- 0.91 | 10 | 1.013 ( 0.085) | 0.965 ( 0.106) | 1.136 ( 0.215) | 0.89- 0.82 | 10 | 1.079 ( 0.054) | 1.037 ( 0.110) | 1.250 ( 0.550) | 0.82- 0.76 | 10 | 0.986 ( 0.062) | 0.936 ( 0.076) | 0.914 ( 0.312) | 0.76- 0.71 | 10 | 1.020 ( 0.044) | 0.980 ( 0.052) | 1.023 ( 0.217) | 0.71- 0.67 | 10 | 0.971 ( 0.038) | 0.914 ( 0.053) | 1.187 ( 0.530) | 0.66- 0.62 | 10 | 0.952 ( 0.073) | 0.877 ( 0.056) | 1.498 ( 0.513) | 0.62- 0.59 | 10 | 0.891 ( 0.054) | 0.838 ( 0.038) | 1.276 ( 0.466) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.51- 0.59 | 100 | 1.009 ( 0.099) | 0.993 ( 0.257) | 1.123 ( 0.455) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 99 obs out of 100 (total:100,skipped:0) (99.00%) UB - matrix: -0.025265 -0.079434 -0.015562 ( 0.000029 0.000009 0.000054 ) 0.072394 -0.029508 0.032882 ( 0.000046 0.000014 0.000084 ) -0.036084 -0.003699 0.076702 ( 0.000047 0.000015 0.000085 ) M - matrix: 0.007181 0.000004 0.000006 ( 0.000008 0.000003 0.000008 ) 0.000004 0.007194 -0.000018 ( 0.000003 0.000002 0.000005 ) 0.000006 -0.000018 0.007207 ( 0.000008 0.000005 0.000014 ) unit cell: 8.370(5) 8.363(2) 8.355(7) 89.86(4) 90.05(6) 90.03(3) V = 584.8(7) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: -0.025306 -0.079318 -0.015710 ( 0.000040 0.000012 0.000072 ) 0.072354 -0.029532 0.032836 ( 0.000049 0.000015 0.000089 ) -0.036187 -0.003666 0.076576 ( 0.000044 0.000014 0.000080 ) M - matrix: 0.007185 0.000003 0.000002 ( 0.000008 0.000004 0.000008 ) 0.000003 0.007177 -0.000004 ( 0.000004 0.000002 0.000006 ) 0.000002 -0.000004 0.007189 ( 0.000008 0.000006 0.000014 ) Constraint UB - matrix: -0.025306 -0.079318 -0.015710 ( 0.000040 0.000012 0.000072 ) 0.072354 -0.029532 0.032836 ( 0.000049 0.000015 0.000089 ) -0.036187 -0.003666 0.076576 ( 0.000044 0.000014 0.000080 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 8.368(6) 8.373(3) 8.366(7) 89.97(5) 90.02(6) 90.03(4) V = 586.1(6) unit cell: 8.3687(7) 8.3687(7) 8.3687(7) 90.0 90.0 90.0 V = 586.11(8) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 274 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025306 -0.079318 -0.015710 ( 0.000040 0.000012 0.000072 ) 0.072354 -0.029532 0.032836 ( 0.000049 0.000015 0.000089 ) -0.036187 -0.003666 0.076576 ( 0.000044 0.000014 0.000080 ) M - matrix: 0.007185 0.000003 0.000002 ( 0.000008 0.000004 0.000008 ) 0.000003 0.007177 -0.000004 ( 0.000004 0.000002 0.000006 ) 0.000002 -0.000004 0.007189 ( 0.000008 0.000006 0.000014 ) Constraint UB - matrix: -0.025306 -0.079318 -0.015710 ( 0.000040 0.000012 0.000072 ) 0.072354 -0.029532 0.032836 ( 0.000049 0.000015 0.000089 ) -0.036187 -0.003666 0.076576 ( 0.000044 0.000014 0.000080 ) M - matrix: 0.007179 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007179 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007179 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 8.368(6) 8.373(3) 8.366(7) 89.97(5) 90.02(6) 90.03(4) V = 586.1(6) unit cell: 8.3687(7) 8.3687(7) 8.3687(7) 90.0 90.0 90.0 V = 586.11(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb 2 of 102 peaks identified as outliers and rejected 100 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 100 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 100 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 1.48 | 10 | 1.051 ( 0.156) | 1.248 ( 0.687) | 0.910 ( 0.340) | 1.41- 1.17 | 10 | 1.087 ( 0.079) | 1.115 ( 0.064) | 0.929 ( 0.296) | 1.17- 1.02 | 10 | 1.059 ( 0.074) | 1.061 ( 0.097) | 1.190 ( 0.492) | 1.01- 0.92 | 10 | 1.016 ( 0.082) | 0.965 ( 0.105) | 1.161 ( 0.370) | 0.92- 0.82 | 10 | 1.060 ( 0.083) | 1.012 ( 0.140) | 1.152 ( 0.435) | 0.82- 0.76 | 10 | 0.988 ( 0.065) | 0.939 ( 0.073) | 1.055 ( 0.507) | 0.76- 0.73 | 10 | 1.019 ( 0.043) | 0.986 ( 0.048) | 1.028 ( 0.214) | 0.71- 0.67 | 10 | 0.979 ( 0.044) | 0.919 ( 0.051) | 1.183 ( 0.536) | 0.67- 0.62 | 10 | 0.962 ( 0.069) | 0.884 ( 0.052) | 1.513 ( 0.486) | 0.62- 0.59 | 10 | 0.898 ( 0.047) | 0.837 ( 0.033) | 1.266 ( 0.470) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 2.52- 0.59 | 100 | 1.012 ( 0.097) | 0.997 ( 0.257) | 1.139 ( 0.458) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.8 | 322 | 1.115 ( 0.118) | 1.237 ( 0.465) | 1.229 ( 1.019) | 12.9-18.5 | 322 | 1.077 ( 0.054) | 1.121 ( 0.240) | 1.170 ( 0.494) | 18.5-22.8 | 322 | 1.063 ( 0.071) | 1.128 ( 0.356) | 1.164 ( 0.538) | 22.9-27.1 | 323 | 1.033 ( 0.084) | 1.081 ( 0.295) | 1.133 ( 0.552) | 27.1-30.6 | 322 | 1.004 ( 0.071) | 1.003 ( 0.246) | 1.199 ( 0.496) | 30.6-33.7 | 322 | 0.975 ( 0.074) | 0.925 ( 0.091) | 1.176 ( 0.511) | 33.8-36.9 | 322 | 0.953 ( 0.069) | 0.903 ( 0.111) | 1.147 ( 0.465) | 36.9-39.7 | 322 | 0.935 ( 0.078) | 0.873 ( 0.138) | 1.203 ( 0.553) | 39.7-42.7 | 322 | 0.918 ( 0.071) | 0.835 ( 0.087) | 1.179 ( 0.526) | 42.7-50.7 | 319 | 0.918 ( 0.082) | 0.809 ( 0.065) | 1.160 ( 0.480) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3218 | 0.999 ( 0.103) | 0.992 ( 0.281) | 1.176 ( 0.585) | Fitted profile normalization line parameters e1 dimension: a=-0.0049 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0017 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:38:11 2018 PROFFITMAIN - Started at Tue Mar 27 16:38:11 2018 OTKP changes: 3208 2 4 6 OTKP changes: 3208 2 4 6 OTKP changes: 3208 2 4 6 No constraint UB - matrix: -0.025055 -0.079511 -0.015610 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029302 0.032928 ( 0.000005 0.000005 0.000006 ) -0.036239 -0.003600 0.076593 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007200 -0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007194 0.000001 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000001 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025055 -0.079511 -0.015610 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029302 0.032928 ( 0.000005 0.000005 0.000006 ) -0.036239 -0.003600 0.076593 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000000 ) UB fit with 3213 obs out of 3218 (total:3218,skipped:0) (99.84%) unit cell: 8.3590(5) 8.3630(5) 8.3624(4) 90.005(5) 90.027(5) 89.981(5) V = 584.58(6) unit cell: 8.36145(13) 8.36145(13) 8.36145(13) 90.0 90.0 90.0 V = 584.581(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024725 -0.079528 -0.015414 ( 0.000014 0.000011 0.000013 ) 0.072526 -0.028885 0.033051 ( 0.000012 0.000010 0.000012 ) -0.036068 -0.003518 0.076551 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007172 -0.000002 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007171 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3753(12) 8.3758(12) 8.3650(12) 90.015(11) 90.137(11) 89.986(11) V = 586.80(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007203 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007217 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3573(11) 8.3642(11) 8.3494(11) 90.049(11) 90.081(11) 89.972(11) V = 583.64(14) unit cell: 8.3570(4) 8.3570(4) 8.3570(4) 90.0 90.0 90.0 V = 583.64(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.725) HKL list info: 806 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007203 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007217 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3573(11) 8.3642(11) 8.3494(11) 90.049(11) 90.081(11) 89.972(11) V = 583.64(14) unit cell: 8.3570(4) 8.3570(4) 8.3570(4) 90.0 90.0 90.0 V = 583.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007203 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007191 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007217 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024709 -0.079638 -0.015551 ( 0.000013 0.000011 0.000013 ) 0.072654 -0.028920 0.033107 ( 0.000012 0.000010 0.000012 ) -0.036250 -0.003584 0.076675 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3573(11) 8.3642(11) 8.3494(11) 90.049(11) 90.081(11) 89.972(11) V = 583.64(14) unit cell: 8.3570(4) 8.3570(4) 8.3570(4) 90.0 90.0 90.0 V = 583.64(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024858 -0.079564 -0.015646 ( 0.000013 0.000015 0.000011 ) 0.072445 -0.029188 0.032942 ( 0.000016 0.000018 0.000013 ) -0.036284 -0.003656 0.076377 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007196 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007163 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3693(14) 8.3617(14) 8.3805(10) 90.033(12) 90.033(12) 89.968(14) V = 586.48(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024992 -0.079538 -0.015503 ( 0.000017 0.000014 0.000012 ) 0.072498 -0.029262 0.033005 ( 0.000012 0.000010 0.000008 ) -0.036257 -0.003621 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000006 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007196 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000010 0.007185 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3621(11) 8.3617(14) 8.3677(11) 89.922(12) 90.046(11) 89.981(12) V = 585.08(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007212 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3522(11) 8.3542(14) 8.3596(11) 89.935(12) 90.003(11) 89.963(12) V = 583.30(15) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.725) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007212 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3522(11) 8.3542(14) 8.3596(11) 89.935(12) 90.003(11) 89.963(12) V = 583.30(15) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007212 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007199 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025032 -0.079609 -0.015461 ( 0.000016 0.000014 0.000012 ) 0.072578 -0.029298 0.032998 ( 0.000011 0.000010 0.000008 ) -0.036301 -0.003554 0.076625 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3522(11) 8.3542(14) 8.3596(11) 89.935(12) 90.003(11) 89.963(12) V = 583.30(15) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025024 -0.079534 -0.015724 ( 0.000008 0.000013 0.000012 ) 0.072418 -0.029342 0.032922 ( 0.000008 0.000014 0.000014 ) -0.036203 -0.003657 0.076529 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3701(11) 8.3592(12) 8.3663(11) 90.038(11) 90.056(11) 89.983(11) V = 585.37(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007212 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3629(10) 8.3524(12) 8.3558(11) 89.995(11) 90.024(10) 90.025(11) V = 583.65(14) unit cell: 8.3570(3) 8.3570(3) 8.3570(3) 90.0 90.0 90.0 V = 583.65(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.725) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007212 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3629(10) 8.3524(12) 8.3558(11) 89.995(11) 90.024(10) 90.025(11) V = 583.65(14) unit cell: 8.3570(3) 8.3570(3) 8.3570(3) 90.0 90.0 90.0 V = 583.65(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007194 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007212 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007206 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025081 -0.079593 -0.015738 ( 0.000008 0.000013 0.000013 ) 0.072422 -0.029376 0.033015 ( 0.000008 0.000014 0.000013 ) -0.036327 -0.003700 0.076604 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3629(10) 8.3524(12) 8.3558(11) 89.995(11) 90.024(10) 90.025(11) V = 583.65(14) unit cell: 8.3570(3) 8.3570(3) 8.3570(3) 90.0 90.0 90.0 V = 583.65(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025241 -0.079454 -0.015761 ( 0.000011 0.000016 0.000017 ) 0.072366 -0.029418 0.032790 ( 0.000008 0.000011 0.000012 ) -0.036259 -0.003621 0.076602 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007189 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3658(10) 8.3642(14) 8.3642(11) 90.082(12) 89.946(10) 90.064(12) V = 585.26(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007204 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007203 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007211 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3569(10) 8.3577(14) 8.3530(11) 90.051(12) 89.990(10) 90.064(12) V = 583.42(14) unit cell: 8.3559(3) 8.3559(3) 8.3559(3) 90.0 90.0 90.0 V = 583.42(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.725) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007204 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007203 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007211 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3569(10) 8.3577(14) 8.3530(11) 90.051(12) 89.990(10) 90.064(12) V = 583.42(14) unit cell: 8.3559(3) 8.3559(3) 8.3559(3) 90.0 90.0 90.0 V = 583.42(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007204 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007203 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007211 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025246 -0.079523 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072495 -0.029415 0.032813 ( 0.000008 0.000011 0.000012 ) -0.036207 -0.003666 0.076718 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3569(10) 8.3577(14) 8.3530(11) 90.051(12) 89.990(10) 90.064(12) V = 583.42(14) unit cell: 8.3559(3) 8.3559(3) 8.3559(3) 90.0 90.0 90.0 V = 583.42(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025307 -0.079446 -0.015634 ( 0.000010 0.000008 0.000010 ) 0.072448 -0.029446 0.032792 ( 0.000014 0.000011 0.000014 ) -0.036123 -0.003535 0.076585 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000005 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000005 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007185 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3626(13) 8.3643(9) 8.3679(12) 90.046(10) 90.039(12) 90.039(10) V = 585.31(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007203 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007208 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3572(13) 8.3591(9) 8.3543(12) 90.068(10) 90.050(12) 90.027(10) V = 583.62(14) unit cell: 8.3569(3) 8.3569(3) 8.3569(3) 90.0 90.0 90.0 V = 583.62(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.725) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007203 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007208 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3572(13) 8.3591(9) 8.3543(12) 90.068(10) 90.050(12) 90.027(10) V = 583.62(14) unit cell: 8.3569(3) 8.3569(3) 8.3569(3) 90.0 90.0 90.0 V = 583.62(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007203 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007200 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007208 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079486 -0.015731 ( 0.000011 0.000008 0.000010 ) 0.072519 -0.029482 0.032794 ( 0.000014 0.000011 0.000014 ) -0.036107 -0.003585 0.076717 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3572(13) 8.3591(9) 8.3543(12) 90.068(10) 90.050(12) 90.027(10) V = 583.62(14) unit cell: 8.3569(3) 8.3569(3) 8.3569(3) 90.0 90.0 90.0 V = 583.62(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb Run 7 has been already processed *** 3D integration started - run 8 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) UB - matrix: -0.025286 -0.079351 -0.015655 ( 0.000040 0.000013 0.000072 ) 0.072366 -0.029504 0.032805 ( 0.000048 0.000015 0.000087 ) -0.036117 -0.003705 0.076668 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007181 0.000005 0.000001 ( 0.000008 0.000004 0.000008 ) 0.000005 0.007181 -0.000010 ( 0.000004 0.000002 0.000006 ) 0.000001 -0.000010 0.007199 ( 0.000008 0.000006 0.000014 ) unit cell: 8.370(5) 8.370(3) 8.360(7) 89.92(5) 90.01(6) 90.04(4) V = 585.7(6) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 No constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007204 0.000001 0.000004 ( 0.000008 0.000004 0.000008 ) 0.000001 0.007194 -0.000007 ( 0.000004 0.000002 0.000006 ) 0.000004 -0.000007 0.007215 ( 0.000008 0.000006 0.000014 ) Constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 8.357(5) 8.363(2) 8.351(7) 89.95(5) 90.03(6) 90.01(4) V = 583.6(6) unit cell: 8.3567(7) 8.3567(7) 8.3567(7) 90.0 90.0 90.0 V = 583.59(8) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.725) HKL list info: 270 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007204 0.000001 0.000004 ( 0.000008 0.000004 0.000008 ) 0.000001 0.007194 -0.000007 ( 0.000004 0.000002 0.000006 ) 0.000004 -0.000007 0.007215 ( 0.000008 0.000006 0.000014 ) Constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 8.357(5) 8.363(2) 8.351(7) 89.95(5) 90.03(6) 90.01(4) V = 583.6(6) unit cell: 8.3567(7) 8.3567(7) 8.3567(7) 90.0 90.0 90.0 V = 583.59(8) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007204 0.000001 0.000004 ( 0.000008 0.000004 0.000008 ) 0.000001 0.007194 -0.000007 ( 0.000004 0.000002 0.000006 ) 0.000004 -0.000007 0.007215 ( 0.000008 0.000006 0.000014 ) Constraint UB - matrix: -0.025304 -0.079427 -0.015658 ( 0.000038 0.000012 0.000069 ) 0.072469 -0.029531 0.032937 ( 0.000049 0.000015 0.000088 ) -0.036223 -0.003623 0.076711 ( 0.000044 0.000014 0.000079 ) M - matrix: 0.007195 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007195 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007195 ( 0.000000 0.000000 0.000001 ) UB fit with 100 obs out of 100 (total:100,skipped:0) (100.00%) unit cell: 8.357(5) 8.363(2) 8.351(7) 89.95(5) 90.03(6) 90.01(4) V = 583.6(6) unit cell: 8.3567(7) 8.3567(7) 8.3567(7) 90.0 90.0 90.0 V = 583.59(8) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=25, width=1.000 - Required frames: #=25, start=1, end=25, - Adjusted required frames (range): #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025057 -0.079470 -0.015589 ( 0.000005 0.000005 0.000006 ) 0.072516 -0.029317 0.032891 ( 0.000006 0.000006 0.000006 ) -0.036255 -0.003633 0.076597 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007201 -0.000003 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007192 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025057 -0.079470 -0.015589 ( 0.000005 0.000005 0.000006 ) 0.072516 -0.029317 0.032891 ( 0.000006 0.000006 0.000006 ) -0.036255 -0.003633 0.076597 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) UB fit with 3213 obs out of 3218 (total:3218,skipped:0) (99.84%) unit cell: 8.3587(6) 8.3661(5) 8.3639(4) 89.970(5) 89.990(5) 89.976(5) V = 584.88(6) unit cell: 8.36287(17) 8.36287(17) 8.36287(17) 90.0 90.0 90.0 V = 584.88(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 76 reflections under beam stop or inside a detector rejection region 24 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_8.rrpprof 4357 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:38:20 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.725) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.725) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.725) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.725) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.725) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.725) PROFFIT INFO: signal sum: min=119.0000 max=23093844.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3188067.7992 PROFFIT INFO: background sum: min=612.0000 max=26230.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=50 max=544 PROFFIT INFO: Inet: min=293.3857 max=5100908.5000 PROFFIT INFO: sig(Inet): min=120.0746 max=47814.8789 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.21 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 59 237 488 895 1012 1860 2952 4013 4357 Percent 0.0 0.0 1.4 5.4 11.2 20.5 23.2 42.7 67.8 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4357 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4357 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100909- 1084928 435 1815171.11 121.34 100.00 1082183- 586699 435 809256.63 100.36 100.00 584371- 250194 435 388447.76 92.95 100.00 250058- 162375 435 194241.24 70.03 100.00 161916- 114358 435 136803.89 48.96 100.00 114192- 86757 435 99606.43 34.95 100.00 86724- 59717 435 73914.29 27.70 100.00 59410- 5199 435 32793.60 18.12 100.00 5120- 2779 435 3673.91 5.16 95.17 2779- 293 442 1969.76 3.59 51.13 ------------------------------------------------------------------------------------ 5100909- 293 4357 355019.74 52.24 94.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 744055.45 91.20 100.00 1.41- 1.12 435 564861.60 64.29 99.31 1.12- 0.96 435 503333.03 69.14 96.78 0.96- 0.87 435 326173.53 57.73 93.56 0.87- 0.81 435 436234.66 67.98 99.08 0.81- 0.73 435 235114.94 40.33 95.63 0.73- 0.71 435 166556.51 33.62 89.43 0.71- 0.65 435 293259.93 45.51 92.18 0.65- 0.62 435 144824.54 26.49 86.44 0.62- 0.58 442 139255.25 26.50 93.21 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 355019.74 52.24 94.56 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:38:20 2018 Sorting 4357 observations 118 unique observations with > 7.00 F2/sig(F2) 4357 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 24 743 Total number of frames 743 Maximum number of 118 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4357 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 3 111 Total number of frames 111 3490 observations > 7.00 F2/sig(F2) 3490 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 3 111 Total number of frames 111 Removing 'redundancy=1' reflections Average redundancy: 26.8 (Out of 3490 removed 4 = 3486, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3486 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 3 111 Total number of frames 111 130 unique data precomputed (should be 130) 130 unique data with 3486 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 26.8 (Out of 3486 removed 0 = 3486, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3486 observations RMS deviation of equivalent data = 0.26445 Rint = 0.20288 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19832, wR= 0.27889 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15807, wR= 0.20834, Acormin=0.580, Acormax=1.324, Acor_av=0.991 F test: Probability=1.000, F= 1.572 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13296, wR= 0.17374, Acormin=0.552, Acormax=1.428, Acor_av=0.936 F test: Probability=1.000, F= 1.412 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13533, wR= 0.18316, Acormin=0.587, Acormax=1.555, Acor_av=0.967 F test: Probability=0.000, F= 0.964 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10761, wR= 0.14589, Acormin=0.487, Acormax=1.561, Acor_av=0.919 F test: Probability=1.000, F= 1.522 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09843, wR= 0.13544, Acormin=0.444, Acormax=1.583, Acor_av=0.926 F test: Probability=1.000, F= 1.193 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12389, wR= 0.16929, Acormin=0.601, Acormax=1.638, Acor_av=0.974 F test: Probability=0.000, F= 0.631 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09832, wR= 0.13566, Acormin=0.494, Acormax=1.655, Acor_av=0.925 F test: Probability=0.505, F= 1.000 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09094, wR= 0.12656, Acormin=0.465, Acormax=1.650, Acor_av=0.932 F test: Probability=1.000, F= 1.167 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08975, wR= 0.12170, Acormin=0.322, Acormax=1.494, Acor_av=0.866 F test: Probability=0.745, F= 1.023 Trying model 10 (ne=8, no=0)... Results: Rint= 0.12134, wR= 0.15770, Acormin=0.425, Acormax=1.435, Acor_av=0.820 F test: Probability=0.000, F= 0.560 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10181, wR= 0.13613, Acormin=0.474, Acormax=1.578, Acor_av=0.884 F test: Probability=0.000, F= 0.795 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10260, wR= 0.13327, Acormin=0.066, Acormax=0.303, Acor_av=0.165 F test: Probability=0.000, F= 0.782 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09504, wR= 0.12472, Acormin=0.063, Acormax=0.327, Acor_av=0.178 F test: Probability=0.000, F= 0.908 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08687, wR= 0.11573, Acormin=0.066, Acormax=0.346, Acor_av=0.187 F test: Probability=0.988, F= 1.082 Final absorption model (ne=6, no=3): Rint= 0.09094, Acormin=0.465, Acormax=1.650, Acor_av=0.932 Combined refinement in use Rint: 0.20299 There are 111 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 147 pars with 10878 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26445 Using Levenberg-Marquardt: 0.00010 New wR= 0.07315 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20288 with corrections 0.05837 Rint for all data: 0.20299 with corrections 0.05859 1 observations identified as outliers and rejected Cycle 2 wR= 0.07310 Using Levenberg-Marquardt: 0.00001 New wR= 0.06663 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20266 with corrections 0.05239 Rint for all data: 0.20299 with corrections 0.05262 0 observations identified as outliers and rejected Cycle 3 wR= 0.06663 Using Levenberg-Marquardt: 0.00000 New wR= 0.06480 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20266 with corrections 0.05075 Rint for all data: 0.20299 with corrections 0.05099 0 observations identified as outliers and rejected Cycle 4 wR= 0.06480 Using Levenberg-Marquardt: 0.00000 New wR= 0.06390 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20266 with corrections 0.04993 Rint for all data: 0.20299 with corrections 0.05017 0 observations identified as outliers and rejected Cycle 5 wR= 0.06390 Using Levenberg-Marquardt: 0.00000 New wR= 0.06341 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20266 with corrections 0.04949 Rint for all data: 0.20299 with corrections 0.04973 0 observations identified as outliers and rejected Final wR= 0.06341 Final frame scales: Min= 0.7127 Max= 1.2873 Final absorption correction factors: Amin= 0.4681 Amax= 1.3806 PROFFIT INFO: Inet (after scale3 abspack): min=627.5803 max=4405245.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=135.4813 max=54266.4805 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4357 reflections read from tmp file 997 reflections are rejected (997 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 1 3 6 4 2 1 7 129 Initial Chi^2= 0.42880 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.84902 Current error model SIG(F2)^2 = 128.11*I_RAW + 0.00*I_BACK+(0.02587*)^2 Cycle 2, Chi^2= 0.99978 Current error model SIG(F2)^2 = 120.81*I_RAW + 0.00*I_BACK+(0.02091*)^2 Cycle 3, Chi^2= 1.00002 Current error model SIG(F2)^2 = 121.80*I_RAW + 0.00*I_BACK+(0.02068*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 121.83*I_RAW + 0.00*I_BACK+(0.02067*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 121.83*I_RAW + 0.00*I_BACK+(0.02067*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4405245- 1043142 435 1687561.77 44.66 100.00 1037931- 569506 435 767164.58 37.04 100.00 569271- 239701 435 377452.22 35.68 100.00 239625- 145449 435 180119.37 30.73 100.00 145426- 116638 435 131293.78 24.71 100.00 116407- 81606 435 95136.64 18.77 100.00 81590- 63325 435 72462.55 15.96 100.00 63248- 4596 435 35614.98 11.26 99.77 4578- 2609 435 3402.68 4.42 93.56 2604- 628 442 1994.72 3.59 66.74 ------------------------------------------------------------------------------------ 4405245- 628 4357 334684.97 22.65 95.96 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 732463.42 36.10 100.00 1.41- 1.12 435 542730.21 28.28 99.54 1.12- 0.96 435 454188.96 27.17 97.24 0.96- 0.87 435 303664.43 23.14 94.94 0.87- 0.81 435 408714.52 26.96 99.31 0.81- 0.73 435 213965.26 18.41 96.55 0.73- 0.71 435 158341.98 17.01 90.80 0.71- 0.65 435 273123.47 21.33 96.09 0.65- 0.62 435 135843.84 13.95 90.34 0.62- 0.58 442 127153.14 14.27 94.80 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 334684.97 22.65 95.96 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 732463.42 36.10 100.00 4.82- 1.12 870 637596.81 32.19 99.77 4.82- 0.96 1305 576460.86 30.52 98.93 4.82- 0.87 1740 508261.76 28.67 97.93 4.82- 0.81 2175 488352.31 28.33 98.21 4.82- 0.73 2610 442621.13 26.67 97.93 4.82- 0.71 3045 402009.83 25.29 96.91 4.82- 0.65 3480 385899.03 24.80 96.81 4.82- 0.62 3915 358115.12 23.59 96.09 4.82- 0.58 4357 334684.97 22.65 95.96 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 334684.97 22.65 95.96 Scale applied to data: s=0.227002 (maximum obs:4405245.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.050; Rsigma 0.028: data 4357 -> merged 157 With outlier rejection... Rint 0.049; Rsigma 0.028: data 4344 -> merged 157 Rejected total: 13, method kkm 10, method Blessing 3 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585518, 4.828307 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 25.86 100.00 362 1.41 - 1.12 14 14 35.64 100.00 499 1.12 - 0.97 14 14 35.71 100.00 500 0.96 - 0.84 14 14 38.29 100.00 536 0.84 - 0.78 14 14 28.86 100.00 404 0.78 - 0.73 14 14 30.93 100.00 433 0.73 - 0.69 14 14 28.07 100.00 393 0.69 - 0.66 14 14 24.43 100.00 342 0.65 - 0.63 14 14 25.50 100.00 357 0.63 - 0.60 14 14 22.36 100.00 313 --------------------------------------------------------------- 8.36 - 0.60 140 140 29.56 100.00 4139 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:38:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.358672 8.366060 8.363892 89.9704 89.9904 89.9763 4344 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2215 0 2913 2912 4344 N (int>3sigma) = 0 0 0 0 2215 0 2798 2790 4168 Mean intensity = 0.0 0.0 0.0 0.0 30.0 0.0 76.1 77.6 75.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.3 0.0 22.7 22.8 22.6 Lattice type: F chosen Volume: 584.88 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.912 5.913 119.95 90.04 119.98 Niggli form: a.a = 34.950 b.b = 34.950 c.c = 34.961 b.c = -17.454 a.c = -0.022 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.032 CUBIC F-lattice R(int) = 0.049 [ 4187] Vol = 584.9 Cell: 8.359 8.366 8.364 90.03 89.99 90.02 Volume: 584.88 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.030 RHOMBOHEDRAL R-lattice R(int) = 0.054 [ 3903] Vol = 438.7 Cell: 5.912 5.912 14.490 89.97 90.05 119.98 Volume: 438.66 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.030 RHOMBOHEDRAL R-lattice R(int) = 0.047 [ 1240] Vol = 438.7 Trigonal Cell: 5.912 5.912 14.490 89.97 90.05 119.98 Volume: 438.66 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.044 TETRAGONAL I-lattice R(int) = 0.048 [ 3937] Vol = 292.4 Cell: 5.913 5.916 8.359 89.98 90.01 90.01 Volume: 292.44 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.030 TETRAGONAL I-lattice R(int) = 0.048 [ 3937] Vol = 292.4 Cell: 5.913 5.916 8.359 89.98 90.01 90.01 Volume: 292.44 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.017 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 3883] Vol = 292.4 Cell: 5.913 8.359 5.916 89.98 89.99 89.99 Volume: 292.44 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.009 MONOCLINIC I-lattice R(int) = 0.046 [ 3529] Vol = 292.4 Cell: 8.359 5.913 5.916 90.01 90.02 89.99 Volume: 292.44 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.024 MONOCLINIC I-lattice R(int) = 0.045 [ 3526] Vol = 292.4 Cell: 5.913 5.912 8.366 90.00 90.04 89.96 Volume: 292.44 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC C-lattice R(int) = 0.045 [ 3540] Vol = 292.4 Cell: 8.359 8.366 5.912 90.00 134.98 90.02 Volume: 292.44 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2851] Vol = 146.2 Cell: 5.912 5.912 5.913 119.95 90.04 119.98 Volume: 146.22 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2215 0 2905 2927 4344 N (int>3sigma) = 0 0 0 0 2215 0 2785 2808 4168 Mean intensity = 0.0 0.0 0.0 0.0 30.0 0.0 75.5 76.9 75.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.3 0.0 22.7 22.7 22.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.164 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 46 46 335 970 N I>3s 45 45 307 970 0.9 0.9 0.7 35.7 8.5 8.5 5.2 26.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.049 3872 Fd-3m 1 1 227 C N N N N 37 2284 0.049 3911 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.358672 8.366060 8.363892 90.0296 89.9904 90.0237 ZERR 3.00 0.000571 0.000540 0.000451 0.0048 0.0050 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3731108- 694362 717 714 26 27.5 1346026.96 42.06 0.043 0.054 677935- 212927 661 658 26 25.3 420302.64 35.67 0.062 0.077 208551- 92087 1005 1005 26 38.7 140104.71 25.51 0.048 0.061 89413- 62466 720 719 26 27.7 76576.55 16.22 0.072 0.094 60795- 3300 549 546 26 21.0 23112.97 8.56 0.086 0.118 3220- 1665 705 702 27 26.0 2502.80 4.09 0.203 0.271 ------------------------------------------------------------------------------------------- 3731108- 1665 4357 4344 157 27.7 333301.75 22.64 0.049 0.062 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 821 815 26 31.3 581346.83 31.46 0.045 0.056 0.023 1.12-0.88 964 963 26 37.0 425243.39 26.28 0.040 0.051 0.026 0.85-0.75 802 802 26 30.8 311871.68 22.16 0.048 0.060 0.030 0.74-0.68 708 706 26 27.2 240355.08 19.60 0.060 0.071 0.034 0.67-0.63 667 667 26 25.7 139036.56 15.41 0.074 0.094 0.043 0.62-0.59 395 391 27 14.5 133009.20 14.07 0.076 0.079 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 4357 4344 157 27.7 333301.75 22.64 0.049 0.062 0.028 inf-0.60 4148 4137 139 29.8 345202.07 23.13 0.048 0.061 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 815 26 26 100.0 31.3 581346.83 190.61 0.045 0.005 1.12-0.88 963 26 26 100.0 37.0 425243.39 162.18 0.040 0.005 0.85-0.75 802 26 26 100.0 30.8 311871.68 129.88 0.048 0.005 0.74-0.68 706 26 26 100.0 27.2 240355.08 103.99 0.060 0.007 0.67-0.63 667 26 26 100.0 25.7 139036.56 77.23 0.074 0.009 0.62-0.59 391 27 27 100.0 14.5 133009.20 61.43 0.076 0.016 -------------------------------------------------------------------------------------------- inf-0.59 4344 157 157 100.0 27.7 333301.75 129.98 0.049 0.006 inf-0.60 4137 139 139 100.0 29.8 345202.07 133.99 0.048 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025057 -0.079470 -0.015589 ( 0.000005 0.000005 0.000006 ) 0.072516 -0.029317 0.032891 ( 0.000006 0.000006 0.000006 ) -0.036255 -0.003633 0.076597 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007201 -0.000003 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007192 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025057 -0.079470 -0.015589 ( 0.000005 0.000005 0.000006 ) 0.072516 -0.029317 0.032891 ( 0.000006 0.000006 0.000006 ) -0.036255 -0.003633 0.076597 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007192 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007192 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007192 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3587(6) 8.3661(5) 8.3639(4) 89.970(5) 89.990(5) 89.976(5) V = 584.88(6) unit cell: 8.36289(17) 8.36289(17) 8.36289(17) 90.0 90.0 90.0 V = 584.88(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.725) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.725) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.725) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.725) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.725) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - -16.000,25 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.725) PROFFIT INFO: signal sum: min=119.0000 max=23093844.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3188067.7992 PROFFIT INFO: background sum: min=612.0000 max=26230.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11956.0000 PROFFIT INFO: num of signal pixels: min=50 max=544 PROFFIT INFO: Inet: min=293.3857 max=5100908.5000 PROFFIT INFO: sig(Inet): min=120.0746 max=47814.8789 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.21 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 118 474 976 1790 2024 3720 5904 8026 8714 Percent 0.0 0.0 1.4 5.4 11.2 20.5 23.2 42.7 67.8 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4357 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4357 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100909- 1084928 435 1815171.11 121.34 100.00 1082183- 586699 435 809256.63 100.36 100.00 584371- 250194 435 388447.76 92.95 100.00 250058- 162375 435 194241.24 70.03 100.00 161916- 114358 435 136803.89 48.96 100.00 114192- 86757 435 99606.43 34.95 100.00 86724- 59717 435 73914.29 27.70 100.00 59410- 5199 435 32793.60 18.12 100.00 5120- 2779 435 3673.91 5.16 95.17 2779- 293 442 1969.76 3.59 51.13 ------------------------------------------------------------------------------------ 5100909- 293 4357 355019.74 52.24 94.56 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 744055.45 91.20 100.00 1.41- 1.12 435 564861.60 64.29 99.31 1.12- 0.96 435 503333.03 69.14 96.78 0.96- 0.87 435 326173.53 57.73 93.56 0.87- 0.81 435 436234.66 67.98 99.08 0.81- 0.73 435 235114.94 40.33 95.63 0.73- 0.71 435 166556.51 33.62 89.43 0.71- 0.65 435 293259.93 45.51 92.18 0.65- 0.62 435 144824.54 26.49 86.44 0.62- 0.58 442 139255.25 26.50 93.21 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 355019.74 52.24 94.56 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:38:22 2018 Sorting 4357 observations 85 unique observations with > 7.00 F2/sig(F2) 4357 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 24 743 Total number of frames 743 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 9 frame = 1 scale 4357 observations in 8 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 8 0 2 84 Total number of frames 84 3490 observations > 7.00 F2/sig(F2) 3490 observations in 8 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 8 0 2 84 Total number of frames 84 Removing 'redundancy=1' reflections Average redundancy: 37.5 (Out of 3490 removed 4 = 3486, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3486 observations in 8 runs Run # start # end # total # 1 0 12 13 2 0 10 24 3 0 11 36 4 0 11 48 5 0 10 59 6 0 11 71 7 0 9 81 8 0 2 84 Total number of frames 84 93 unique data precomputed (should be 93) 93 unique data with 3486 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 37.5 (Out of 3486 removed 0 = 3486, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3486 observations RMS deviation of equivalent data = 0.26507 Rint = 0.20314 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19847, wR= 0.27943 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15813, wR= 0.20819, Acormin=0.580, Acormax=1.324, Acor_av=0.991 F test: Probability=1.000, F= 1.573 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13299, wR= 0.17382, Acormin=0.552, Acormax=1.428, Acor_av=0.936 F test: Probability=1.000, F= 1.413 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13523, wR= 0.18308, Acormin=0.588, Acormax=1.552, Acor_av=0.968 F test: Probability=0.000, F= 0.965 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10739, wR= 0.14598, Acormin=0.487, Acormax=1.560, Acor_av=0.920 F test: Probability=1.000, F= 1.529 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09825, wR= 0.13581, Acormin=0.442, Acormax=1.582, Acor_av=0.926 F test: Probability=1.000, F= 1.192 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12356, wR= 0.16922, Acormin=0.602, Acormax=1.636, Acor_av=0.977 F test: Probability=0.000, F= 0.632 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09812, wR= 0.13564, Acormin=0.498, Acormax=1.649, Acor_av=0.927 F test: Probability=0.510, F= 1.001 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09075, wR= 0.12684, Acormin=0.464, Acormax=1.657, Acor_av=0.934 F test: Probability=1.000, F= 1.168 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08988, wR= 0.12193, Acormin=0.325, Acormax=1.496, Acor_av=0.867 F test: Probability=0.676, F= 1.016 Trying model 10 (ne=8, no=0)... Results: Rint= 0.12092, wR= 0.15755, Acormin=0.431, Acormax=1.424, Acor_av=0.822 F test: Probability=0.000, F= 0.562 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10148, wR= 0.13607, Acormin=0.479, Acormax=1.568, Acor_av=0.886 F test: Probability=0.000, F= 0.797 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10250, wR= 0.13366, Acormin=0.066, Acormax=0.302, Acor_av=0.164 F test: Probability=0.000, F= 0.780 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09517, wR= 0.12511, Acormin=0.064, Acormax=0.325, Acor_av=0.178 F test: Probability=0.000, F= 0.902 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08716, wR= 0.11622, Acormin=0.065, Acormax=0.343, Acor_av=0.185 F test: Probability=0.974, F= 1.070 Final absorption model (ne=6, no=3): Rint= 0.09075, Acormin=0.464, Acormax=1.657, Acor_av=0.934 Combined refinement in use Rint: 0.20325 There are 84 active scales (one needs to be fixed) Refinement control: frame scale #26 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 120 pars with 7260 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26507 Using Levenberg-Marquardt: 0.00010 New wR= 0.07733 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20314 with corrections 0.06134 Rint for all data: 0.20325 with corrections 0.06156 1 observations identified as outliers and rejected Cycle 2 wR= 0.07727 Using Levenberg-Marquardt: 0.00001 New wR= 0.07011 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20292 with corrections 0.05524 Rint for all data: 0.20325 with corrections 0.05550 1 observations identified as outliers and rejected Cycle 3 wR= 0.07018 Using Levenberg-Marquardt: 0.00000 New wR= 0.06770 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20296 with corrections 0.05308 Rint for all data: 0.20325 with corrections 0.05333 0 observations identified as outliers and rejected Cycle 4 wR= 0.06770 Using Levenberg-Marquardt: 0.00000 New wR= 0.06632 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20296 with corrections 0.05188 Rint for all data: 0.20325 with corrections 0.05212 0 observations identified as outliers and rejected Cycle 5 wR= 0.06632 Using Levenberg-Marquardt: 0.00000 New wR= 0.06545 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20296 with corrections 0.05112 Rint for all data: 0.20325 with corrections 0.05136 0 observations identified as outliers and rejected Final wR= 0.06545 Final frame scales: Min= 0.7436 Max= 1.2796 Final absorption correction factors: Amin= 0.4667 Amax= 1.3883 PROFFIT INFO: Inet (after scale3 abspack): min=638.0435 max=4416498.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=135.1263 max=53759.6602 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4357 reflections read from tmp file 1010 reflections are rejected (1009 as outliers, 1 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 0 3 2 2 2 1 3 1 95 Initial Chi^2= 0.42814 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.89348 Current error model SIG(F2)^2 = 141.70*I_RAW + 0.00*I_BACK+(0.02255*)^2 Cycle 2, Chi^2= 1.00040 Current error model SIG(F2)^2 = 115.84*I_RAW + 0.00*I_BACK+(0.02336*)^2 Cycle 3, Chi^2= 1.00004 Current error model SIG(F2)^2 = 117.44*I_RAW + 0.00*I_BACK+(0.02305*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 117.25*I_RAW + 0.00*I_BACK+(0.02309*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 117.25*I_RAW + 0.00*I_BACK+(0.02309*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4416499- 1035018 435 1686137.68 40.79 100.00 1032235- 568943 435 767561.19 34.79 100.00 568941- 238533 435 377469.33 33.60 100.00 238390- 145727 435 179996.19 29.51 100.00 145643- 116456 435 131589.87 24.20 100.00 116220- 81629 435 95233.73 18.71 100.00 81598- 63244 435 72468.10 15.97 100.00 63170- 4587 435 35570.79 11.33 99.77 4578- 2612 435 3398.72 4.47 94.48 2610- 638 442 1995.86 3.67 69.23 ------------------------------------------------------------------------------------ 4416499- 638 4357 334606.91 21.67 96.30 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 731119.56 33.43 100.00 1.41- 1.12 435 542656.56 26.56 99.54 1.12- 0.96 435 453735.57 25.73 97.47 0.96- 0.87 435 304121.41 22.20 95.63 0.87- 0.81 435 408833.77 25.76 99.54 0.81- 0.73 435 214023.01 17.85 96.78 0.73- 0.71 435 158586.72 16.72 91.26 0.71- 0.65 435 273265.66 20.74 96.55 0.65- 0.62 435 135657.18 13.76 91.03 0.62- 0.58 442 127403.96 14.12 95.25 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 334606.91 21.67 96.30 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 435 731119.56 33.43 100.00 4.82- 1.12 870 636888.06 29.99 99.77 4.82- 0.96 1305 575837.23 28.57 99.00 4.82- 0.87 1740 507908.27 26.98 98.16 4.82- 0.81 2175 488093.37 26.74 98.44 4.82- 0.73 2610 442414.98 25.26 98.16 4.82- 0.71 3045 401868.08 24.04 97.18 4.82- 0.65 3480 385792.78 23.62 97.10 4.82- 0.62 3915 357999.94 22.53 96.42 4.82- 0.58 4357 334606.91 21.67 96.30 ------------------------------------------------------------------------------------ 4.82- 0.58 4357 334606.91 21.67 96.30 Scale applied to data: s=0.226423 (maximum obs:4416498.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.051; Rsigma 0.030: data 4357 -> merged 110 With outlier rejection... Rint 0.051; Rsigma 0.030: data 4345 -> merged 110 Rejected total: 12, method kkm 9, method Blessing 3 Completeness direct cell (a, b, c) = (8.363, 8.363, 8.363), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585519, 4.828317 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 27.50 100.00 275 1.61 - 1.21 10 10 40.50 100.00 405 1.17 - 1.01 10 10 51.70 100.00 517 0.99 - 0.89 10 10 50.00 100.00 500 0.88 - 0.81 10 10 48.00 100.00 480 0.81 - 0.74 10 10 42.00 100.00 420 0.73 - 0.71 10 10 46.00 100.00 460 0.70 - 0.66 10 10 38.40 100.00 384 0.66 - 0.64 10 10 35.80 100.00 358 0.63 - 0.60 10 10 34.10 100.00 341 --------------------------------------------------------------- 8.36 - 0.60 100 100 41.40 100.00 4140 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:38:21 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.358672 8.366060 8.363892 89.9704 89.9904 89.9763 4344 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.64 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2215 0 2913 2912 4344 N (int>3sigma) = 0 0 0 0 2215 0 2798 2790 4168 Mean intensity = 0.0 0.0 0.0 0.0 30.0 0.0 76.1 77.6 75.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.3 0.0 22.7 22.8 22.6 Lattice type: F chosen Volume: 584.88 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Unitcell: 5.912 5.912 5.913 119.95 90.04 119.98 Niggli form: a.a = 34.950 b.b = 34.950 c.c = 34.961 b.c = -17.454 a.c = -0.022 a.b = -17.466 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.032 CUBIC F-lattice R(int) = 0.049 [ 4187] Vol = 584.9 Cell: 8.359 8.366 8.364 90.03 89.99 90.02 Volume: 584.88 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.030 RHOMBOHEDRAL R-lattice R(int) = 0.054 [ 3903] Vol = 438.7 Cell: 5.912 5.912 14.490 89.97 90.05 119.98 Volume: 438.66 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.030 RHOMBOHEDRAL R-lattice R(int) = 0.047 [ 1240] Vol = 438.7 Trigonal Cell: 5.912 5.912 14.490 89.97 90.05 119.98 Volume: 438.66 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 -0.5000 -1.0000 -1.0000 -1.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.044 TETRAGONAL I-lattice R(int) = 0.048 [ 3937] Vol = 292.4 Cell: 5.913 5.916 8.359 89.98 90.01 90.01 Volume: 292.44 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.030 TETRAGONAL I-lattice R(int) = 0.048 [ 3937] Vol = 292.4 Cell: 5.913 5.916 8.359 89.98 90.01 90.01 Volume: 292.44 Matrix: 0.0000 0.5000 -0.5000 0.0000 -0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.017 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 3883] Vol = 292.4 Cell: 5.913 8.359 5.916 89.98 89.99 89.99 Volume: 292.44 Matrix: 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 0.0000 -0.5000 -0.5000 ------------------------------------------------------------------------------ Option: [17] err= 0.009 MONOCLINIC I-lattice R(int) = 0.046 [ 3529] Vol = 292.4 Cell: 8.359 5.913 5.916 90.01 90.02 89.99 Volume: 292.44 Matrix:-1.0000 0.0000 0.0000 0.0000 -0.5000 0.5000 0.0000 0.5000 0.5000 ------------------------------------------------------------------------------ Option: [39] err= 0.024 MONOCLINIC I-lattice R(int) = 0.045 [ 3526] Vol = 292.4 Cell: 5.913 5.912 8.366 90.00 90.04 89.96 Volume: 292.44 Matrix: 0.5000 0.0000 0.5000 -0.5000 0.0000 0.5000 0.0000 -1.0000 0.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.032 MONOCLINIC C-lattice R(int) = 0.045 [ 3540] Vol = 292.4 Cell: 8.359 8.366 5.912 90.00 134.98 90.02 Volume: 292.44 Matrix:-1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 2851] Vol = 146.2 Cell: 5.912 5.912 5.913 119.95 90.04 119.98 Volume: 146.22 Matrix: 0.5000 0.0000 -0.5000 -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2215 0 2905 2927 4344 N (int>3sigma) = 0 0 0 0 2215 0 2785 2808 4168 Mean intensity = 0.0 0.0 0.0 0.0 30.0 0.0 75.5 76.9 75.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.3 0.0 22.7 22.7 22.6 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.164 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 46 46 335 970 N I>3s 45 45 307 970 0.9 0.9 0.7 35.7 8.5 8.5 5.2 26.1 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.049 3872 Fd-3m 1 1 227 C N N N N 37 2284 0.049 3911 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.358672 8.366060 8.363892 90.0296 89.9904 90.0237 ZERR 3.00 0.000571 0.000540 0.000451 0.0048 0.0050 0.0054 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3704900- 486919 967 964 27 35.7 1152949.01 36.98 0.048 0.061 466386- 112527 1281 1279 27 47.4 200212.54 28.61 0.054 0.070 99745- 33389 1077 1076 27 39.9 73570.72 16.09 0.071 0.094 9847- 1750 1032 1026 29 35.4 3286.74 4.46 0.173 0.233 ------------------------------------------------------------------------------------------- 3704900- 1750 4357 4345 110 39.5 333728.19 21.67 0.051 0.065 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1110 1103 27 40.9 598888.18 30.12 0.046 0.059 0.025 1.01-0.78 1263 1262 27 46.7 324358.76 21.91 0.044 0.055 0.030 0.78-0.65 1220 1220 29 42.1 218265.09 17.63 0.061 0.081 0.036 0.65-0.59 764 760 27 28.1 149804.13 15.46 0.077 0.087 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 4357 4345 110 39.5 333728.19 21.67 0.051 0.065 0.030 inf-0.60 4148 4138 99 41.8 345617.65 22.11 0.050 0.064 0.030 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1103 27 27 100.0 40.9 598888.18 216.08 0.046 0.005 1.01-0.78 1262 27 27 100.0 46.7 324358.76 161.26 0.044 0.005 0.78-0.65 1220 29 29 100.0 42.1 218265.09 120.20 0.061 0.006 0.65-0.59 760 27 27 100.0 28.1 149804.13 94.51 0.077 0.012 -------------------------------------------------------------------------------------------- inf-0.59 4345 110 110 100.0 39.5 333728.19 151.97 0.051 0.006 inf-0.60 4138 99 99 100.0 41.8 345617.65 156.08 0.050 0.006 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:44:52 2018) ID: 2932; threads 39; handles 876; mem 518924.00 (1237720.00)kB; time: 1w 5d 1h 50m 22s MEMORY INFO: Memory PF:0.0, Ph:232.0, V:1208.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:506.8,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:232.0, V:1210.0; MEMORY INFO: Process info - Handles: 877, Memory: PF:508.6,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:44:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) 8.37024 ( 0.00057 ) 8.37691 ( 0.00054 ) 8.37554 ( 0.00045 ) 90.02113 ( 0.00484 ) 90.03240 ( 0.00501 ) 90.03043 ( 0.00537 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\plots_red\xs1714a_absscaleint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleintcorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscaleres.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_absscalerescorr.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bfactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_afactor.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_cover.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_hklplot.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_resolutionstats.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_rint.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2bm.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_chi2am.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_stickabsorption.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_incidence.dat) DELETE INFO: Deleting grl file... (D:\Data\xs1714a\xs1714a.grl) DELETE INFO: Deleting ins file... (D:\Data\xs1714a\xs1714a.ins) DELETE INFO: Deleting eqv file... (D:\Data\xs1714a\xs1714a.eqv) DELETE INFO: Deleting hkl file... (D:\Data\xs1714a\xs1714a.hkl) DELETE INFO: Deleting hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting p4p file... (D:\Data\xs1714a\xs1714a.p4p) DELETE INFO: Deleting p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) DELETE INFO: Deleting rint file... (D:\Data\xs1714a\xs1714a.rint) DELETE INFO: Deleting rint_redun file... (D:\Data\xs1714a\xs1714a.rint_redun) DELETE INFO: Deleting errmod file... (D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:44:52 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000006 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007201 -0.000003 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007192 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(5) 8.3755(4) 90.021(5) 90.032(5) 90.030(5) V = 587.27(6) unit cell: 8.36289(17) 8.36289(17) 8.36289(17) 90.0 90.0 90.0 V = 584.88(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 452 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 445 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 445 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.981 ( 0.174) | 1.324 ( 0.739) | 1.557 ( 2.296) | 1.33- 1.09 | 45 | 1.069 ( 0.114) | 1.092 ( 0.140) | 1.111 ( 0.488) | 1.09- 0.94 | 45 | 1.056 ( 0.114) | 1.073 ( 0.140) | 1.073 ( 0.398) | 0.94- 0.84 | 45 | 1.078 ( 0.108) | 1.069 ( 0.142) | 1.142 ( 0.397) | 0.84- 0.78 | 45 | 1.104 ( 0.100) | 1.016 ( 0.119) | 1.376 ( 0.505) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.985 ( 0.124) | 1.369 ( 0.513) | 0.73- 0.69 | 45 | 1.088 ( 0.080) | 0.931 ( 0.104) | 1.361 ( 0.510) | 0.69- 0.65 | 45 | 1.065 ( 0.069) | 0.888 ( 0.098) | 1.304 ( 0.446) | 0.65- 0.62 | 45 | 1.049 ( 0.078) | 0.846 ( 0.047) | 1.390 ( 0.609) | 0.62- 0.59 | 40 | 1.021 ( 0.082) | 0.806 ( 0.034) | 1.400 ( 0.563) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 445 | 1.062 ( 0.111) | 1.005 ( 0.294) | 1.307 ( 0.880) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 444 obs out of 445 (total:445,skipped:0) (99.78%) UB - matrix: -0.024577 -0.079438 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072473 -0.028947 0.032942 ( 0.000013 0.000011 0.000013 ) -0.036035 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000025 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000025 0.007160 0.000008 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000008 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3856(13) 8.3828(12) 8.3816(14) 90.068(12) 90.083(13) 89.803(12) V = 589.18(16) OTKP changes: 444 1 1 1 No constraint UB - matrix: -0.024649 -0.079493 -0.015423 ( 0.000012 0.000010 0.000012 ) 0.072534 -0.028812 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036124 -0.003521 0.076555 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079493 -0.015423 ( 0.000012 0.000010 0.000012 ) 0.072534 -0.028812 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036124 -0.003521 0.076555 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) unit cell: 8.3745(12) 8.3816(11) 8.3656(12) 90.041(11) 90.079(12) 89.974(11) V = 587.19(14) unit cell: 8.3739(4) 8.3739(4) 8.3739(4) 90.0 90.0 90.0 V = 587.19(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.915) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079493 -0.015423 ( 0.000012 0.000010 0.000012 ) 0.072534 -0.028812 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036124 -0.003521 0.076555 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079493 -0.015423 ( 0.000012 0.000010 0.000012 ) 0.072534 -0.028812 0.033021 ( 0.000013 0.000011 0.000012 ) -0.036124 -0.003521 0.076555 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) unit cell: 8.3745(12) 8.3816(11) 8.3656(12) 90.041(11) 90.079(12) 89.974(11) V = 587.19(14) unit cell: 8.3739(4) 8.3739(4) 8.3739(4) 90.0 90.0 90.0 V = 587.19(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 448 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.986 ( 0.169) | 1.298 ( 0.707) | 1.555 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.087 ( 0.140) | 1.155 ( 0.505) | 1.09- 0.96 | 44 | 1.063 ( 0.105) | 1.084 ( 0.143) | 1.117 ( 0.479) | 0.96- 0.84 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.145 ( 0.403) | 0.84- 0.81 | 44 | 1.112 ( 0.099) | 1.034 ( 0.130) | 1.356 ( 0.480) | 0.81- 0.73 | 44 | 1.087 ( 0.089) | 0.989 ( 0.129) | 1.292 ( 0.473) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.949 ( 0.114) | 1.392 ( 0.482) | 0.70- 0.67 | 44 | 1.077 ( 0.072) | 0.883 ( 0.071) | 1.434 ( 0.478) | 0.67- 0.63 | 44 | 1.073 ( 0.063) | 0.870 ( 0.063) | 1.463 ( 0.597) | 0.63- 0.59 | 44 | 1.011 ( 0.080) | 0.807 ( 0.036) | 1.267 ( 0.484) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 440 | 1.064 ( 0.108) | 1.006 ( 0.282) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 39 | 1.034 ( 0.140) | 1.212 ( 0.488) | 1.144 ( 0.710) | 1.41- 1.17 | 39 | 1.017 ( 0.109) | 1.175 ( 0.516) | 1.084 ( 0.530) | 1.17- 0.99 | 39 | 1.025 ( 0.094) | 1.047 ( 0.109) | 0.944 ( 0.361) | 0.99- 0.89 | 39 | 1.018 ( 0.096) | 1.012 ( 0.121) | 1.026 ( 0.379) | 0.89- 0.82 | 39 | 1.019 ( 0.086) | 1.008 ( 0.096) | 1.145 ( 0.483) | 0.82- 0.75 | 39 | 1.007 ( 0.087) | 0.964 ( 0.126) | 1.064 ( 0.402) | 0.75- 0.71 | 39 | 0.968 ( 0.066) | 0.899 ( 0.082) | 1.221 ( 0.547) | 0.71- 0.67 | 39 | 0.965 ( 0.044) | 0.877 ( 0.053) | 1.246 ( 0.535) | 0.67- 0.63 | 39 | 0.948 ( 0.039) | 0.830 ( 0.043) | 1.280 ( 0.452) | 0.63- 0.59 | 43 | 0.909 ( 0.040) | 0.782 ( 0.038) | 1.129 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 394 | 0.990 ( 0.094) | 0.978 ( 0.273) | 1.128 ( 0.501) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 8 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb PROFFITPEAK info: 595 peaks in the peak location table UB fit with 263 obs out of 296 (total:296,skipped:0) (88.85%) UB - matrix: -0.025370 -0.079312 -0.015747 ( 0.000048 0.000025 0.000072 ) 0.072477 -0.029463 0.032939 ( 0.000051 0.000027 0.000076 ) -0.036194 -0.003702 0.076649 ( 0.000049 0.000026 0.000073 ) M - matrix: 0.007207 0.000011 0.000013 ( 0.000009 0.000005 0.000008 ) 0.000011 0.007172 -0.000005 ( 0.000005 0.000004 0.000006 ) 0.000013 -0.000005 0.007208 ( 0.000008 0.000006 0.000012 ) unit cell: 8.355(5) 8.375(3) 8.355(6) 89.96(5) 90.10(6) 90.09(4) V = 584.6(6) UB fit with 263 obs out of 296 (total:296,skipped:0) (88.85%) UB - matrix: -0.025370 -0.079312 -0.015747 ( 0.000048 0.000025 0.000072 ) 0.072477 -0.029463 0.032939 ( 0.000051 0.000027 0.000076 ) -0.036194 -0.003702 0.076649 ( 0.000049 0.000026 0.000073 ) M - matrix: 0.007207 0.000011 0.000013 ( 0.000009 0.000005 0.000008 ) 0.000011 0.007172 -0.000005 ( 0.000005 0.000004 0.000006 ) 0.000013 -0.000005 0.007208 ( 0.000008 0.000006 0.000012 ) unit cell: 8.355(5) 8.375(3) 8.355(6) 89.96(5) 90.10(6) 90.09(4) V = 584.6(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 UB - matrix: -0.025453 -0.079285 -0.015831 ( 0.000045 0.000024 0.000067 ) 0.072460 -0.029512 0.033014 ( 0.000050 0.000027 0.000075 ) -0.036244 -0.003652 0.076648 ( 0.000049 0.000026 0.000073 ) M - matrix: 0.007212 0.000012 0.000017 ( 0.000008 0.000004 0.000008 ) 0.000012 0.007170 0.000001 ( 0.000004 0.000004 0.000006 ) 0.000017 0.000001 0.007215 ( 0.000008 0.000006 0.000012 ) UB fit with 264 obs out of 296 (total:296,skipped:0) (89.19%) unit cell: 8.352(5) 8.376(3) 8.350(6) 90.01(5) 90.14(6) 90.10(4) V = 584.2(6) UB fit with 264 obs out of 296 (total:296,skipped:0) (89.19%) UB - matrix: -0.025453 -0.079285 -0.015831 ( 0.000045 0.000024 0.000067 ) 0.072460 -0.029512 0.033014 ( 0.000050 0.000027 0.000075 ) -0.036244 -0.003652 0.076648 ( 0.000049 0.000026 0.000073 ) M - matrix: 0.007212 0.000012 0.000017 ( 0.000008 0.000004 0.000008 ) 0.000012 0.007170 0.000001 ( 0.000004 0.000004 0.000006 ) 0.000017 0.000001 0.007215 ( 0.000008 0.000006 0.000012 ) unit cell: 8.352(5) 8.376(3) 8.350(6) 90.01(5) 90.14(6) 90.10(4) V = 584.2(6) OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 OTKP changes: 50 1 1 1 296 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Run 8 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 426 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025453 -0.079285 -0.015831 ( 0.000045 0.000024 0.000067 ) 0.072460 -0.029512 0.033014 ( 0.000050 0.000027 0.000075 ) -0.036244 -0.003652 0.076648 ( 0.000049 0.000026 0.000073 ) M - matrix: 0.007212 0.000012 0.000017 ( 0.000008 0.000004 0.000008 ) 0.000012 0.007170 0.000001 ( 0.000004 0.000004 0.000006 ) 0.000017 0.000001 0.007215 ( 0.000008 0.000006 0.000012 ) UB fit with 264 obs out of 296 (total:296,skipped:0) (89.19%) unit cell: 8.352(5) 8.376(3) 8.350(6) 90.01(5) 90.14(6) 90.10(4) V = 584.2(6) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 264 obs out of 296 (total:296,skipped:0) (89.19%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb 5 of 221 peaks identified as outliers and rejected 216 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 216 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 216 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 22 | 1.033 ( 0.134) | 1.130 ( 0.485) | 1.066 ( 0.461) | 1.41- 1.15 | 22 | 1.079 ( 0.128) | 1.166 ( 0.471) | 1.188 ( 0.518) | 1.12- 0.98 | 22 | 1.055 ( 0.092) | 1.039 ( 0.120) | 1.072 ( 0.447) | 0.96- 0.89 | 22 | 1.021 ( 0.081) | 0.972 ( 0.121) | 1.128 ( 0.386) | 0.89- 0.82 | 22 | 1.052 ( 0.069) | 1.019 ( 0.106) | 1.098 ( 0.554) | 0.82- 0.75 | 22 | 1.018 ( 0.061) | 0.982 ( 0.097) | 1.186 ( 0.495) | 0.75- 0.71 | 22 | 0.987 ( 0.051) | 0.928 ( 0.087) | 0.983 ( 0.284) | 0.70- 0.66 | 22 | 0.974 ( 0.044) | 0.893 ( 0.047) | 1.269 ( 0.493) | 0.64- 0.62 | 22 | 0.929 ( 0.049) | 0.856 ( 0.046) | 1.343 ( 0.549) | 0.62- 0.59 | 18 | 0.897 ( 0.055) | 0.840 ( 0.042) | 1.264 ( 0.544) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 216 | 1.006 ( 0.099) | 0.985 ( 0.252) | 1.158 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 215 obs out of 216 (total:216,skipped:0) (99.54%) UB - matrix: -0.025337 -0.079433 -0.015668 ( 0.000022 0.000012 0.000030 ) 0.072407 -0.029483 0.032890 ( 0.000023 0.000013 0.000032 ) -0.036080 -0.003715 0.076691 ( 0.000025 0.000014 0.000035 ) M - matrix: 0.007187 0.000012 0.000011 ( 0.000004 0.000002 0.000003 ) 0.000012 0.007193 -0.000010 ( 0.000002 0.000002 0.000003 ) 0.000011 -0.000010 0.007209 ( 0.000003 0.000003 0.000006 ) unit cell: 8.367(2) 8.3635(15) 8.354(3) 89.92(2) 90.09(3) 90.095(19) V = 584.6(3) OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 No constraint UB - matrix: -0.025320 -0.079327 -0.015737 ( 0.000023 0.000012 0.000031 ) 0.072343 -0.029545 0.032877 ( 0.000024 0.000013 0.000033 ) -0.036206 -0.003645 0.076576 ( 0.000021 0.000012 0.000029 ) M - matrix: 0.007185 0.000003 0.000004 ( 0.000004 0.000002 0.000003 ) 0.000003 0.007179 -0.000002 ( 0.000002 0.000002 0.000003 ) 0.000004 -0.000002 0.007192 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.025320 -0.079327 -0.015737 ( 0.000023 0.000012 0.000031 ) 0.072343 -0.029545 0.032877 ( 0.000024 0.000013 0.000033 ) -0.036206 -0.003645 0.076576 ( 0.000021 0.000012 0.000029 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 8.368(2) 8.3714(16) 8.364(3) 89.98(2) 90.04(2) 90.03(2) V = 585.9(3) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.86(5) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 429 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025320 -0.079327 -0.015737 ( 0.000023 0.000012 0.000031 ) 0.072343 -0.029545 0.032877 ( 0.000024 0.000013 0.000033 ) -0.036206 -0.003645 0.076576 ( 0.000021 0.000012 0.000029 ) M - matrix: 0.007185 0.000003 0.000004 ( 0.000004 0.000002 0.000003 ) 0.000003 0.007179 -0.000002 ( 0.000002 0.000002 0.000003 ) 0.000004 -0.000002 0.007192 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.025320 -0.079327 -0.015737 ( 0.000023 0.000012 0.000031 ) 0.072343 -0.029545 0.032877 ( 0.000024 0.000013 0.000033 ) -0.036206 -0.003645 0.076576 ( 0.000021 0.000012 0.000029 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) unit cell: 8.368(2) 8.3714(16) 8.364(3) 89.98(2) 90.04(2) 90.03(2) V = 585.9(3) unit cell: 8.3676(4) 8.3676(4) 8.3676(4) 90.0 90.0 90.0 V = 585.86(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 216 obs out of 216 (total:216,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb 5 of 220 peaks identified as outliers and rejected 215 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 215 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 215 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.41 | 22 | 1.034 ( 0.134) | 1.134 ( 0.485) | 1.055 ( 0.403) | 1.41- 1.15 | 22 | 1.083 ( 0.134) | 1.166 ( 0.476) | 1.237 ( 0.496) | 1.15- 0.97 | 22 | 1.042 ( 0.100) | 1.028 ( 0.124) | 1.023 ( 0.435) | 0.97- 0.89 | 22 | 1.019 ( 0.087) | 0.956 ( 0.115) | 1.216 ( 0.413) | 0.88- 0.82 | 22 | 1.049 ( 0.073) | 1.021 ( 0.100) | 1.092 ( 0.578) | 0.81- 0.75 | 22 | 1.021 ( 0.057) | 0.980 ( 0.098) | 1.200 ( 0.488) | 0.73- 0.70 | 22 | 0.989 ( 0.049) | 0.936 ( 0.081) | 0.996 ( 0.329) | 0.69- 0.64 | 22 | 0.972 ( 0.046) | 0.884 ( 0.041) | 1.253 ( 0.551) | 0.64- 0.62 | 22 | 0.928 ( 0.049) | 0.860 ( 0.048) | 1.280 ( 0.508) | 0.62- 0.59 | 17 | 0.907 ( 0.050) | 0.843 ( 0.037) | 1.296 ( 0.538) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 215 | 1.007 ( 0.099) | 0.984 ( 0.253) | 1.162 ( 0.490) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.8 | 333 | 1.117 ( 0.118) | 1.240 ( 0.471) | 1.235 ( 1.007) | 12.8-18.5 | 333 | 1.078 ( 0.053) | 1.121 ( 0.237) | 1.177 ( 0.498) | 18.5-22.8 | 333 | 1.064 ( 0.070) | 1.126 ( 0.350) | 1.172 ( 0.538) | 22.8-27.1 | 333 | 1.033 ( 0.083) | 1.078 ( 0.291) | 1.136 ( 0.552) | 27.1-30.6 | 333 | 1.005 ( 0.070) | 1.003 ( 0.242) | 1.192 ( 0.493) | 30.6-33.7 | 333 | 0.973 ( 0.074) | 0.926 ( 0.091) | 1.163 ( 0.506) | 33.7-36.9 | 333 | 0.953 ( 0.068) | 0.903 ( 0.110) | 1.143 ( 0.463) | 36.9-39.7 | 333 | 0.935 ( 0.077) | 0.870 ( 0.128) | 1.205 ( 0.549) | 39.7-42.6 | 333 | 0.918 ( 0.070) | 0.838 ( 0.099) | 1.179 ( 0.535) | 42.6-50.7 | 335 | 0.918 ( 0.082) | 0.809 ( 0.065) | 1.160 ( 0.478) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3332 | 0.999 ( 0.103) | 0.991 ( 0.280) | 1.176 ( 0.583) | Fitted profile normalization line parameters e1 dimension: a=-0.0050 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0017 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708023 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:45:29 2018 PROFFITMAIN - Started at Tue Mar 27 16:45:29 2018 OTKP changes: 3322 2 4 6 OTKP changes: 3322 2 4 6 OTKP changes: 3322 2 4 6 No constraint UB - matrix: -0.025061 -0.079502 -0.015616 ( 0.000005 0.000005 0.000005 ) 0.072525 -0.029313 0.032934 ( 0.000005 0.000005 0.000005 ) -0.036240 -0.003607 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007201 -0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000003 0.007193 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000000 0.007196 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025061 -0.079502 -0.015616 ( 0.000005 0.000005 0.000005 ) 0.072525 -0.029313 0.032934 ( 0.000005 0.000005 0.000005 ) -0.036240 -0.003607 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000000 ) UB fit with 3327 obs out of 3332 (total:3332,skipped:0) (99.85%) unit cell: 8.3584(5) 8.3634(5) 8.3613(4) 89.998(4) 90.030(4) 89.977(5) V = 584.50(6) unit cell: 8.36105(13) 8.36105(13) 8.36105(13) 90.0 90.0 90.0 V = 584.496(16) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) UB - matrix: -0.024723 -0.079527 -0.015414 ( 0.000014 0.000011 0.000013 ) 0.072525 -0.028882 0.033050 ( 0.000012 0.000010 0.000012 ) -0.036069 -0.003518 0.076551 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007172 -0.000002 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007171 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3755(12) 8.3760(12) 8.3651(12) 90.016(11) 90.135(11) 89.986(11) V = 586.83(14) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 No constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007192 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3568(12) 8.3636(11) 8.3489(11) 90.050(11) 90.081(11) 89.972(11) V = 583.53(14) unit cell: 8.3564(4) 8.3564(4) 8.3564(4) 90.0 90.0 90.0 V = 583.53(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.719) HKL list info: 805 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007192 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3568(12) 8.3636(11) 8.3489(11) 90.050(11) 90.081(11) 89.972(11) V = 583.53(14) unit cell: 8.3564(4) 8.3564(4) 8.3564(4) 90.0 90.0 90.0 V = 583.53(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007192 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079642 -0.015555 ( 0.000013 0.000011 0.000013 ) 0.072658 -0.028924 0.033110 ( 0.000012 0.000010 0.000012 ) -0.036254 -0.003586 0.076679 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3568(12) 8.3636(11) 8.3489(11) 90.050(11) 90.081(11) 89.972(11) V = 583.53(14) unit cell: 8.3564(4) 8.3564(4) 8.3564(4) 90.0 90.0 90.0 V = 583.53(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024857 -0.079563 -0.015644 ( 0.000013 0.000015 0.000011 ) 0.072445 -0.029186 0.032941 ( 0.000016 0.000018 0.000013 ) -0.036283 -0.003656 0.076379 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007195 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3693(14) 8.3618(14) 8.3804(10) 90.032(12) 90.032(12) 89.967(14) V = 586.48(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024994 -0.079538 -0.015503 ( 0.000017 0.000014 0.000012 ) 0.072496 -0.029264 0.033003 ( 0.000011 0.000010 0.000008 ) -0.036257 -0.003620 0.076525 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000006 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007196 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000006 -0.000010 0.007186 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3621(11) 8.3617(14) 8.3676(11) 89.923(12) 90.044(11) 89.982(12) V = 585.07(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007200 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3517(11) 8.3537(14) 8.3590(11) 89.935(12) 90.002(11) 89.963(12) V = 583.19(15) unit cell: 8.3548(3) 8.3548(3) 8.3548(3) 90.0 90.0 90.0 V = 583.19(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.719) HKL list info: 785 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007200 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3517(11) 8.3537(14) 8.3590(11) 89.935(12) 90.002(11) 89.963(12) V = 583.19(15) unit cell: 8.3548(3) 8.3548(3) 8.3548(3) 90.0 90.0 90.0 V = 583.19(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007209 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007200 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079614 -0.015459 ( 0.000016 0.000014 0.000012 ) 0.072584 -0.029298 0.033000 ( 0.000011 0.000010 0.000008 ) -0.036303 -0.003551 0.076631 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3517(11) 8.3537(14) 8.3590(11) 89.935(12) 90.002(11) 89.963(12) V = 583.19(15) unit cell: 8.3548(3) 8.3548(3) 8.3548(3) 90.0 90.0 90.0 V = 583.19(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025027 -0.079532 -0.015725 ( 0.000008 0.000013 0.000012 ) 0.072417 -0.029342 0.032923 ( 0.000008 0.000014 0.000014 ) -0.036205 -0.003657 0.076530 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007200 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3700(11) 8.3593(12) 8.3662(11) 90.038(11) 90.055(11) 89.984(11) V = 585.36(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3623(10) 8.3519(12) 8.3553(11) 89.994(11) 90.024(10) 90.025(11) V = 583.54(14) unit cell: 8.3565(3) 8.3565(3) 8.3565(3) 90.0 90.0 90.0 V = 583.54(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.719) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3623(10) 8.3519(12) 8.3553(11) 89.994(11) 90.024(10) 90.025(11) V = 583.54(14) unit cell: 8.3565(3) 8.3565(3) 8.3565(3) 90.0 90.0 90.0 V = 583.54(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079599 -0.015739 ( 0.000008 0.000013 0.000013 ) 0.072426 -0.029376 0.033020 ( 0.000008 0.000014 0.000013 ) -0.036331 -0.003701 0.076607 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3623(10) 8.3519(12) 8.3553(11) 89.994(11) 90.024(10) 90.025(11) V = 583.54(14) unit cell: 8.3565(3) 8.3565(3) 8.3565(3) 90.0 90.0 90.0 V = 583.54(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025242 -0.079454 -0.015759 ( 0.000011 0.000016 0.000017 ) 0.072368 -0.029418 0.032789 ( 0.000008 0.000011 0.000012 ) -0.036257 -0.003622 0.076602 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007189 0.000008 -0.000007 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000007 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3657(10) 8.3642(14) 8.3642(11) 90.080(12) 89.947(10) 90.064(12) V = 585.25(15) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3564(10) 8.3572(14) 8.3525(11) 90.051(12) 89.991(10) 90.064(12) V = 583.30(14) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.719) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3564(10) 8.3572(14) 8.3525(11) 90.051(12) 89.991(10) 90.064(12) V = 583.30(14) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079529 -0.015756 ( 0.000011 0.000016 0.000017 ) 0.072501 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036208 -0.003669 0.076724 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3564(10) 8.3572(14) 8.3525(11) 90.051(12) 89.991(10) 90.064(12) V = 583.30(14) unit cell: 8.3553(3) 8.3553(3) 8.3553(3) 90.0 90.0 90.0 V = 583.30(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025307 -0.079445 -0.015635 ( 0.000010 0.000008 0.000010 ) 0.072448 -0.029448 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036123 -0.003536 0.076587 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000005 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000005 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007185 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3627(13) 8.3643(9) 8.3677(12) 90.045(10) 90.038(12) 90.038(10) V = 585.30(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007204 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007209 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3567(13) 8.3586(9) 8.3537(12) 90.068(10) 90.051(12) 90.027(10) V = 583.51(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.51(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.719) HKL list info: 792 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007204 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007209 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3567(13) 8.3586(9) 8.3537(12) 90.068(10) 90.051(12) 90.027(10) V = 583.51(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.51(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007204 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007209 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025312 -0.079492 -0.015733 ( 0.000011 0.000008 0.000010 ) 0.072525 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003587 0.076723 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3567(13) 8.3586(9) 8.3537(12) 90.068(10) 90.051(12) 90.027(10) V = 583.51(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.51(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb Run 7 has been already processed *** 3D integration started - run 8 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) UB - matrix: -0.025326 -0.079347 -0.015708 ( 0.000023 0.000012 0.000031 ) 0.072362 -0.029508 0.032835 ( 0.000024 0.000013 0.000033 ) -0.036154 -0.003691 0.076613 ( 0.000023 0.000012 0.000031 ) M - matrix: 0.007185 0.000008 0.000004 ( 0.000004 0.000002 0.000003 ) 0.000008 0.007180 -0.000005 ( 0.000002 0.000002 0.000003 ) 0.000004 -0.000005 0.007194 ( 0.000003 0.000003 0.000005 ) unit cell: 8.368(2) 8.3706(16) 8.362(3) 89.96(2) 90.03(3) 90.06(2) V = 585.7(3) OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 OTKP changes: 215 1 1 1 No constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007204 0.000003 0.000003 ( 0.000004 0.000002 0.000003 ) 0.000003 0.007195 -0.000002 ( 0.000002 0.000002 0.000003 ) 0.000003 -0.000002 0.007211 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 8.357(2) 8.3622(16) 8.353(3) 89.98(2) 90.02(3) 90.02(2) V = 583.7(3) unit cell: 8.3574(4) 8.3574(4) 8.3574(4) 90.0 90.0 90.0 V = 583.73(5) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.719) HKL list info: 422 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007204 0.000003 0.000003 ( 0.000004 0.000002 0.000003 ) 0.000003 0.007195 -0.000002 ( 0.000002 0.000002 0.000003 ) 0.000003 -0.000002 0.007211 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 8.357(2) 8.3622(16) 8.353(3) 89.98(2) 90.02(3) 90.02(2) V = 583.7(3) unit cell: 8.3574(4) 8.3574(4) 8.3574(4) 90.0 90.0 90.0 V = 583.73(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007204 0.000003 0.000003 ( 0.000004 0.000002 0.000003 ) 0.000003 0.007195 -0.000002 ( 0.000002 0.000002 0.000003 ) 0.000003 -0.000002 0.007211 ( 0.000003 0.000003 0.000005 ) Constraint UB - matrix: -0.025326 -0.079432 -0.015693 ( 0.000022 0.000012 0.000031 ) 0.072444 -0.029535 0.032926 ( 0.000024 0.000013 0.000033 ) -0.036255 -0.003603 0.076683 ( 0.000022 0.000012 0.000030 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 215 obs out of 215 (total:215,skipped:0) (100.00%) unit cell: 8.357(2) 8.3622(16) 8.353(3) 89.98(2) 90.02(3) 90.02(2) V = 583.7(3) unit cell: 8.3574(4) 8.3574(4) 8.3574(4) 90.0 90.0 90.0 V = 583.73(5) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=50, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025061 -0.079465 -0.015592 ( 0.000005 0.000005 0.000005 ) 0.072520 -0.029333 0.032901 ( 0.000006 0.000006 0.000006 ) -0.036258 -0.003633 0.076601 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007202 -0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025061 -0.079465 -0.015592 ( 0.000005 0.000005 0.000005 ) 0.072520 -0.029333 0.032901 ( 0.000006 0.000006 0.000006 ) -0.036258 -0.003633 0.076601 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) UB fit with 3327 obs out of 3332 (total:3332,skipped:0) (99.85%) unit cell: 8.3581(6) 8.3659(5) 8.3630(4) 89.965(5) 89.995(5) 89.968(5) V = 584.77(6) unit cell: 8.36235(17) 8.36235(17) 8.36235(17) 90.0 90.0 90.0 V = 584.77(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 78 reflections under beam stop or inside a detector rejection region 25 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_8.rrpprof 4510 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:45:38 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.719) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.719) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.719) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.719) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.719) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.719) PROFFIT INFO: signal sum: min=119.0000 max=23100528.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3187892.7273 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=561 PROFFIT INFO: Inet: min=293.3857 max=5100628.5000 PROFFIT INFO: sig(Inet): min=120.1885 max=47844.0234 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 62 248 508 928 1050 1929 3053 4155 4510 Percent 0.0 0.0 1.4 5.5 11.3 20.6 23.3 42.8 67.7 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4510 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4510 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100629- 1079396 451 1809063.83 121.46 100.00 1078873- 580492 451 802948.25 99.83 100.00 578736- 246285 451 383412.83 92.89 100.00 245909- 160698 451 193419.89 69.30 100.00 160435- 113442 451 135805.40 49.00 100.00 113417- 86289 451 99021.53 34.87 100.00 86249- 58488 451 72970.04 27.56 100.00 58407- 5054 451 31874.16 17.64 100.00 5040- 2748 451 3612.24 5.12 94.68 2739- 293 451 1951.45 3.60 50.33 ------------------------------------------------------------------------------------ 5100629- 293 4510 353407.96 52.13 94.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 746341.96 90.83 100.00 1.41- 1.12 451 551698.08 65.07 99.33 1.12- 0.96 451 511374.40 69.09 96.67 0.96- 0.87 451 324072.86 57.47 93.35 0.87- 0.81 451 430453.78 67.36 99.11 0.81- 0.73 451 231908.45 40.03 95.57 0.73- 0.71 451 165293.07 33.24 88.25 0.71- 0.65 451 289541.29 45.11 92.46 0.65- 0.62 451 145016.90 26.80 87.36 0.62- 0.58 451 138378.82 26.27 92.90 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 353407.96 52.13 94.50 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:45:39 2018 Sorting 4510 observations 119 unique observations with > 7.00 F2/sig(F2) 4510 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 49 768 Total number of frames 768 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4510 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 7 115 Total number of frames 115 3610 observations > 7.00 F2/sig(F2) 3610 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 6 114 Total number of frames 114 Removing 'redundancy=1' reflections Average redundancy: 27.7 (Out of 3610 removed 4 = 3606, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3606 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 6 114 Total number of frames 114 130 unique data precomputed (should be 130) 130 unique data with 3606 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 27.7 (Out of 3606 removed 0 = 3606, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3606 observations RMS deviation of equivalent data = 0.26143 Rint = 0.20166 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19728, wR= 0.27516 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15941, wR= 0.20920, Acormin=0.593, Acormax=1.323, Acor_av=0.989 F test: Probability=1.000, F= 1.529 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13178, wR= 0.17220, Acormin=0.558, Acormax=1.425, Acor_av=0.942 F test: Probability=1.000, F= 1.462 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13778, wR= 0.18470, Acormin=0.579, Acormax=1.543, Acor_av=0.963 F test: Probability=0.000, F= 0.913 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10642, wR= 0.14438, Acormin=0.491, Acormax=1.562, Acor_av=0.925 F test: Probability=1.000, F= 1.529 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09865, wR= 0.13494, Acormin=0.439, Acormax=1.575, Acor_av=0.927 F test: Probability=1.000, F= 1.161 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12753, wR= 0.17143, Acormin=0.591, Acormax=1.608, Acor_av=0.967 F test: Probability=0.000, F= 0.598 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09789, wR= 0.13474, Acormin=0.493, Acormax=1.653, Acor_av=0.927 F test: Probability=0.655, F= 1.014 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09129, wR= 0.12617, Acormin=0.460, Acormax=1.643, Acor_av=0.932 F test: Probability=1.000, F= 1.163 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08938, wR= 0.12043, Acormin=0.328, Acormax=1.502, Acor_av=0.870 F test: Probability=0.875, F= 1.040 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11893, wR= 0.15483, Acormin=0.441, Acormax=1.446, Acor_av=0.832 F test: Probability=0.000, F= 0.588 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10050, wR= 0.13407, Acormin=0.478, Acormax=1.584, Acor_av=0.892 F test: Probability=0.000, F= 0.823 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10187, wR= 0.13232, Acormin=0.067, Acormax=0.308, Acor_av=0.169 F test: Probability=0.000, F= 0.799 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09409, wR= 0.12343, Acormin=0.064, Acormax=0.333, Acor_av=0.184 F test: Probability=0.000, F= 0.934 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08616, wR= 0.11458, Acormin=0.068, Acormax=0.354, Acor_av=0.192 F test: Probability=0.999, F= 1.109 Final absorption model (ne=6, no=3): Rint= 0.09129, Acormin=0.460, Acormax=1.643, Acor_av=0.932 Combined refinement in use Rint: 0.20178 There are 114 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 150 pars with 11325 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26143 Using Levenberg-Marquardt: 0.00010 New wR= 0.07364 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20166 with corrections 0.05864 Rint for all data: 0.20178 with corrections 0.05886 1 observations identified as outliers and rejected Cycle 2 wR= 0.07360 Using Levenberg-Marquardt: 0.00001 New wR= 0.06695 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20145 with corrections 0.05272 Rint for all data: 0.20178 with corrections 0.05298 0 observations identified as outliers and rejected Cycle 3 wR= 0.06695 Using Levenberg-Marquardt: 0.00000 New wR= 0.06502 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20145 with corrections 0.05114 Rint for all data: 0.20178 with corrections 0.05138 0 observations identified as outliers and rejected Cycle 4 wR= 0.06502 Using Levenberg-Marquardt: 0.00000 New wR= 0.06412 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20145 with corrections 0.05044 Rint for all data: 0.20178 with corrections 0.05069 0 observations identified as outliers and rejected Cycle 5 wR= 0.06412 Using Levenberg-Marquardt: 0.00000 New wR= 0.06366 There are 1 clusters with unrefined scales (size 1-1) Rint for refined data: 0.20145 with corrections 0.05007 Rint for all data: 0.20178 with corrections 0.05031 1 observations identified as outliers and rejected Final wR= 0.06366 Final frame scales: Min= 0.7144 Max= 1.3299 Final absorption correction factors: Amin= 0.4692 Amax= 1.3880 PROFFIT INFO: Inet (after scale3 abspack): min=610.0813 max=4389187.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=136.2080 max=53704.0703 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4510 reflections read from tmp file 1038 reflections are rejected (1038 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 1 3 4 4 5 2 4 130 Initial Chi^2= 0.43989 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.85041 Current error model SIG(F2)^2 = 128.11*I_RAW + 0.00*I_BACK+(0.02713*)^2 Cycle 2, Chi^2= 1.00015 Current error model SIG(F2)^2 = 121.58*I_RAW + 0.00*I_BACK+(0.02197*)^2 Cycle 3, Chi^2= 1.00000 Current error model SIG(F2)^2 = 121.76*I_RAW + 0.00*I_BACK+(0.02193*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 121.76*I_RAW + 0.00*I_BACK+(0.02193*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4389188- 1033854 451 1685064.71 42.51 100.00 1033732- 563312 451 761275.57 35.64 100.00 562163- 239212 451 373580.97 34.42 100.00 239035- 144587 451 179838.53 29.94 100.00 144571- 115320 451 130510.95 24.21 100.00 115294- 81323 451 94478.95 18.55 100.00 81247- 62617 451 71822.55 15.73 100.00 62563- 4502 451 34547.69 10.97 99.78 4493- 2571 451 3355.91 4.40 93.35 2571- 610 451 1981.92 3.57 65.41 ------------------------------------------------------------------------------------ 4389188- 610 4510 333645.77 21.99 95.85 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 735588.37 34.67 100.00 1.41- 1.12 451 534405.13 27.14 99.56 1.12- 0.96 451 459749.99 26.48 97.34 0.96- 0.87 451 302115.97 22.46 94.68 0.87- 0.81 451 403386.04 26.05 99.33 0.81- 0.73 451 211213.24 17.94 96.67 0.73- 0.71 451 157133.54 16.54 89.80 0.71- 0.65 451 269868.06 20.75 96.23 0.65- 0.62 451 136153.61 13.93 90.69 0.62- 0.58 451 126843.78 13.97 94.24 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 333645.77 21.99 95.85 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 735588.37 34.67 100.00 4.82- 1.12 902 634996.75 30.91 99.78 4.82- 0.96 1353 576581.16 29.43 98.97 4.82- 0.87 1804 507964.87 27.69 97.89 4.82- 0.81 2255 487049.10 27.36 98.18 4.82- 0.73 2706 441076.46 25.79 97.93 4.82- 0.71 3157 400513.19 24.47 96.77 4.82- 0.65 3608 384182.54 24.01 96.70 4.82- 0.62 4059 356623.77 22.89 96.03 4.82- 0.58 4510 333645.77 21.99 95.85 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 333645.77 21.99 95.85 Scale applied to data: s=0.227832 (maximum obs:4389187.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.050; Rsigma 0.029: data 4510 -> merged 157 With outlier rejection... Rint 0.050; Rsigma 0.029: data 4499 -> merged 157 Rejected total: 11, method kkm 9, method Blessing 2 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585481, 4.828003 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 26.86 100.00 376 1.41 - 1.12 14 14 37.14 100.00 520 1.12 - 0.97 14 14 36.86 100.00 516 0.96 - 0.84 14 14 39.36 100.00 551 0.84 - 0.78 14 14 30.00 100.00 420 0.78 - 0.73 14 14 31.86 100.00 446 0.73 - 0.69 14 14 29.14 100.00 408 0.69 - 0.65 14 14 25.14 100.00 352 0.65 - 0.63 14 14 26.43 100.00 370 0.63 - 0.60 14 14 23.29 100.00 326 --------------------------------------------------------------- 8.36 - 0.60 140 140 30.61 100.00 4285 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:45:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.358073 8.365926 8.363044 89.9650 89.9950 89.9679 4499 Reflections read from file xs1714a.hkl; mean (I/sigma) = 21.99 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2295 0 3016 3020 4499 N (int>3sigma) = 0 0 0 0 2295 0 2894 2891 4312 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.2 77.8 75.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 22.0 22.1 22.0 Lattice type: F chosen Volume: 584.77 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.911 5.912 5.912 90.03 119.95 119.98 Niggli form: a.a = 34.942 b.b = 34.946 c.c = 34.953 b.c = -0.021 a.c = -17.445 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.050 [ 4342] Vol = 584.8 Cell: 8.363 8.366 8.358 90.03 90.00 90.03 Volume: 584.77 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.042 RHOMBOHEDRAL R-lattice R(int) = 0.055 [ 4058] Vol = 438.6 Cell: 5.913 5.912 14.490 90.03 90.03 120.01 Volume: 438.58 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.042 RHOMBOHEDRAL R-lattice R(int) = 0.049 [ 1293] Vol = 438.6 Trigonal Cell: 5.913 5.912 14.490 90.03 90.03 120.01 Volume: 438.58 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.019 TETRAGONAL I-lattice R(int) = 0.049 [ 4092] Vol = 292.4 Cell: 5.916 5.913 8.358 89.98 89.97 89.98 Volume: 292.38 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.042 TETRAGONAL I-lattice R(int) = 0.049 [ 4092] Vol = 292.4 Cell: 5.913 5.916 8.358 90.03 90.02 89.98 Volume: 292.38 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4038] Vol = 292.4 Cell: 5.913 5.916 8.358 89.97 89.98 89.98 Volume: 292.38 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.027 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4034] Vol = 292.4 Cell: 5.911 8.363 5.914 89.97 89.95 89.98 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.013 MONOCLINIC I-lattice R(int) = 0.047 [ 3684] Vol = 292.4 Cell: 5.916 5.913 8.358 90.02 90.03 89.98 Volume: 292.38 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.032 MONOCLINIC I-lattice R(int) = 0.045 [ 3682] Vol = 292.4 Cell: 5.911 5.914 8.363 90.03 90.02 89.95 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC I-lattice R(int) = 0.045 [ 3697] Vol = 292.4 Cell: 5.911 8.363 5.914 89.97 90.05 90.02 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.027 MONOCLINIC I-lattice R(int) = 0.045 [ 3680] Vol = 292.4 Cell: 5.914 5.911 8.363 89.98 90.03 90.05 Volume: 292.38 Matrix: 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.026 MONOCLINIC C-lattice R(int) = 0.045 [ 3681] Vol = 292.4 Cell: 10.240 5.912 5.912 90.03 125.22 89.98 Volume: 292.38 Matrix: 0.5000 -1.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.042 [ 3006] Vol = 146.2 Cell: 5.911 5.912 5.912 90.03 119.95 119.98 Volume: 146.19 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2295 0 3016 3029 4499 N (int>3sigma) = 0 0 0 0 2295 0 2894 2903 4312 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.2 76.2 75.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 22.0 22.1 22.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 47 47 345 1007 N I>3s 46 46 315 1007 0.9 0.9 0.7 35.9 8.5 8.5 5.1 25.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.050 4017 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4056 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363044 8.365926 8.358073 90.0321 89.9950 90.0350 ZERR 3.00 0.000446 0.000521 0.000564 0.0053 0.0049 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3733729- 690569 740 739 26 28.4 1347479.85 40.20 0.044 0.056 676770- 212965 687 683 26 26.3 417694.96 34.44 0.064 0.078 208330- 92230 1042 1042 26 40.1 139728.76 25.00 0.048 0.062 89063- 62101 742 742 26 28.5 76180.19 16.05 0.074 0.097 60442- 3193 595 592 26 22.8 22073.02 8.26 0.088 0.117 3178- 1702 704 701 27 26.0 2471.71 4.08 0.205 0.275 ------------------------------------------------------------------------------------------- 3733729- 1702 4510 4499 157 28.7 332962.04 21.99 0.050 0.063 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 852 847 26 32.6 583339.61 30.28 0.047 0.059 0.024 1.12-0.88 994 993 26 38.2 427180.04 25.50 0.039 0.051 0.027 0.85-0.75 831 831 26 32.0 308453.84 21.54 0.049 0.061 0.031 0.74-0.68 732 730 26 28.1 238980.78 19.19 0.061 0.072 0.035 0.67-0.63 690 690 26 26.5 138161.21 15.14 0.076 0.096 0.044 0.62-0.59 411 408 27 15.1 131385.91 13.77 0.079 0.081 0.045 ------------------------------------------------------------------------------------------------------ inf-0.59 4510 4499 157 28.7 332962.04 21.99 0.050 0.063 0.029 inf-0.60 4292 4283 139 30.8 345072.51 22.47 0.049 0.062 0.029 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 847 26 26 100.0 32.6 583339.61 187.44 0.047 0.005 1.12-0.88 993 26 26 100.0 38.2 427180.04 160.19 0.039 0.005 0.85-0.75 831 26 26 100.0 32.0 308453.84 128.66 0.049 0.005 0.74-0.68 730 26 26 100.0 28.1 238980.78 103.86 0.061 0.007 0.67-0.63 690 26 26 100.0 26.5 138161.21 77.30 0.076 0.009 0.62-0.59 408 27 27 100.0 15.1 131385.91 61.78 0.079 0.016 -------------------------------------------------------------------------------------------- inf-0.59 4499 157 157 100.0 28.7 332962.04 128.72 0.050 0.007 inf-0.60 4283 139 139 100.0 30.8 345072.51 132.69 0.049 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025061 -0.079465 -0.015592 ( 0.000005 0.000005 0.000005 ) 0.072520 -0.029333 0.032901 ( 0.000006 0.000006 0.000006 ) -0.036258 -0.003633 0.076601 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007202 -0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007193 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025061 -0.079465 -0.015592 ( 0.000005 0.000005 0.000005 ) 0.072520 -0.029333 0.032901 ( 0.000006 0.000006 0.000006 ) -0.036258 -0.003633 0.076601 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3581(6) 8.3659(5) 8.3630(4) 89.965(5) 89.995(5) 89.968(5) V = 584.77(6) unit cell: 8.36235(17) 8.36235(17) 8.36235(17) 90.0 90.0 90.0 V = 584.77(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.719) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.719) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.719) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.719) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.719) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 9.000,50 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.719) PROFFIT INFO: signal sum: min=119.0000 max=23100528.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3187892.7273 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=561 PROFFIT INFO: Inet: min=293.3857 max=5100628.5000 PROFFIT INFO: sig(Inet): min=120.1885 max=47844.0234 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.14 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 124 496 1016 1856 2100 3858 6106 8310 9020 Percent 0.0 0.0 1.4 5.5 11.3 20.6 23.3 42.8 67.7 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4510 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4510 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5100629- 1079396 451 1809063.83 121.46 100.00 1078873- 580492 451 802948.25 99.83 100.00 578736- 246285 451 383412.83 92.89 100.00 245909- 160698 451 193419.89 69.30 100.00 160435- 113442 451 135805.40 49.00 100.00 113417- 86289 451 99021.53 34.87 100.00 86249- 58488 451 72970.04 27.56 100.00 58407- 5054 451 31874.16 17.64 100.00 5040- 2748 451 3612.24 5.12 94.68 2739- 293 451 1951.45 3.60 50.33 ------------------------------------------------------------------------------------ 5100629- 293 4510 353407.96 52.13 94.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 746341.96 90.83 100.00 1.41- 1.12 451 551698.08 65.07 99.33 1.12- 0.96 451 511374.40 69.09 96.67 0.96- 0.87 451 324072.86 57.47 93.35 0.87- 0.81 451 430453.78 67.36 99.11 0.81- 0.73 451 231908.45 40.03 95.57 0.73- 0.71 451 165293.07 33.24 88.25 0.71- 0.65 451 289541.29 45.11 92.46 0.65- 0.62 451 145016.90 26.80 87.36 0.62- 0.58 451 138378.82 26.27 92.90 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 353407.96 52.13 94.50 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:45:40 2018 Sorting 4510 observations 85 unique observations with > 7.00 F2/sig(F2) 4510 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 49 768 Total number of frames 768 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4510 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 4 78 Total number of frames 78 3610 observations > 7.00 F2/sig(F2) 3610 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 4 78 Total number of frames 78 Removing 'redundancy=1' reflections Average redundancy: 38.8 (Out of 3610 removed 4 = 3606, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3606 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 4 78 Total number of frames 78 93 unique data precomputed (should be 93) 93 unique data with 3606 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 38.8 (Out of 3606 removed 0 = 3606, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3606 observations RMS deviation of equivalent data = 0.26200 Rint = 0.20194 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19782, wR= 0.27568 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15982, wR= 0.20927, Acormin=0.594, Acormax=1.322, Acor_av=0.989 F test: Probability=1.000, F= 1.530 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13208, wR= 0.17242, Acormin=0.559, Acormax=1.425, Acor_av=0.942 F test: Probability=1.000, F= 1.463 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13798, wR= 0.18486, Acormin=0.581, Acormax=1.540, Acor_av=0.963 F test: Probability=0.000, F= 0.915 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10643, wR= 0.14467, Acormin=0.492, Acormax=1.560, Acor_av=0.925 F test: Probability=1.000, F= 1.536 Trying model 5 (ne=4, no=3)... Results: Rint= 0.09857, wR= 0.13529, Acormin=0.438, Acormax=1.573, Acor_av=0.927 F test: Probability=1.000, F= 1.163 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12749, wR= 0.17164, Acormin=0.593, Acormax=1.602, Acor_av=0.970 F test: Probability=0.000, F= 0.597 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09788, wR= 0.13497, Acormin=0.497, Acormax=1.647, Acor_av=0.928 F test: Probability=0.643, F= 1.013 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09129, wR= 0.12652, Acormin=0.464, Acormax=1.650, Acor_av=0.933 F test: Probability=1.000, F= 1.162 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08967, wR= 0.12069, Acormin=0.331, Acormax=1.500, Acor_av=0.871 F test: Probability=0.831, F= 1.033 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11866, wR= 0.15501, Acormin=0.448, Acormax=1.429, Acor_av=0.834 F test: Probability=0.000, F= 0.591 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10028, wR= 0.13420, Acormin=0.483, Acormax=1.569, Acor_av=0.894 F test: Probability=0.000, F= 0.826 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10176, wR= 0.13265, Acormin=0.068, Acormax=0.307, Acor_av=0.169 F test: Probability=0.000, F= 0.801 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09419, wR= 0.12381, Acormin=0.065, Acormax=0.333, Acor_av=0.183 F test: Probability=0.000, F= 0.932 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08637, wR= 0.11490, Acormin=0.068, Acormax=0.352, Acor_av=0.191 F test: Probability=0.998, F= 1.103 Final absorption model (ne=6, no=3): Rint= 0.09129, Acormin=0.464, Acormax=1.650, Acor_av=0.933 Combined refinement in use Rint: 0.20206 There are 78 active scales (one needs to be fixed) Refinement control: frame scale #58 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 3 (37 parameters) Refinement control: 114 pars with 6555 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.26200 Using Levenberg-Marquardt: 0.00010 New wR= 0.07948 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20194 with corrections 0.06320 Rint for all data: 0.20206 with corrections 0.06342 1 observations identified as outliers and rejected Cycle 2 wR= 0.07940 Using Levenberg-Marquardt: 0.00001 New wR= 0.07155 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20173 with corrections 0.05626 Rint for all data: 0.20206 with corrections 0.05652 1 observations identified as outliers and rejected Cycle 3 wR= 0.07162 Using Levenberg-Marquardt: 0.00000 New wR= 0.06904 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20177 with corrections 0.05407 Rint for all data: 0.20206 with corrections 0.05431 0 observations identified as outliers and rejected Cycle 4 wR= 0.06904 Using Levenberg-Marquardt: 0.00000 New wR= 0.06767 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20177 with corrections 0.05303 Rint for all data: 0.20206 with corrections 0.05325 0 observations identified as outliers and rejected Cycle 5 wR= 0.06767 Using Levenberg-Marquardt: 0.00000 New wR= 0.06679 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20177 with corrections 0.05237 Rint for all data: 0.20206 with corrections 0.05257 0 observations identified as outliers and rejected Final wR= 0.06679 Final frame scales: Min= 0.7660 Max= 1.2894 Final absorption correction factors: Amin= 0.4595 Amax= 1.4193 PROFFIT INFO: Inet (after scale3 abspack): min=630.5247 max=4366447.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=132.9640 max=52390.3086 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4510 reflections read from tmp file 1091 reflections are rejected (1091 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 2 4 2 1 0 2 2 95 Initial Chi^2= 0.43361 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88190 Current error model SIG(F2)^2 = 143.78*I_RAW + 0.00*I_BACK+(0.02218*)^2 Cycle 2, Chi^2= 0.99999 Current error model SIG(F2)^2 = 122.71*I_RAW + 0.00*I_BACK+(0.02163*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 122.71*I_RAW + 0.00*I_BACK+(0.02163*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4366448- 1033883 451 1685355.93 42.99 100.00 1033055- 562667 451 761647.15 35.90 100.00 562519- 237948 451 373154.16 34.61 100.00 236824- 144702 451 179856.54 30.17 100.00 144700- 114746 451 130837.64 24.19 100.00 114743- 81276 451 94618.22 18.55 100.00 81191- 62315 451 71749.58 15.72 100.00 62298- 4488 451 34458.12 10.93 99.78 4483- 2570 451 3356.05 4.37 92.90 2569- 631 451 1981.65 3.57 65.19 ------------------------------------------------------------------------------------ 4366448- 631 4510 333701.50 22.10 95.79 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 734568.24 34.99 100.00 1.41- 1.12 451 534511.33 27.32 99.33 1.12- 0.96 451 459996.98 26.67 97.34 0.96- 0.87 451 302692.67 22.56 94.68 0.87- 0.81 451 403337.80 26.18 99.33 0.81- 0.73 451 211416.64 17.99 96.45 0.73- 0.71 451 157868.61 16.56 89.80 0.71- 0.65 451 269720.12 20.80 96.01 0.65- 0.62 451 136018.37 13.94 90.69 0.62- 0.58 451 126884.26 13.97 94.24 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 333701.50 22.10 95.79 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 451 734568.24 34.99 100.00 4.82- 1.12 902 634539.78 31.16 99.67 4.82- 0.96 1353 576358.85 29.66 98.89 4.82- 0.87 1804 507942.30 27.89 97.84 4.82- 0.81 2255 487021.40 27.54 98.14 4.82- 0.73 2706 441087.28 25.95 97.86 4.82- 0.71 3157 400627.47 24.61 96.71 4.82- 0.65 3608 384264.05 24.13 96.62 4.82- 0.62 4059 356681.20 23.00 95.96 4.82- 0.58 4510 333701.50 22.10 95.79 ------------------------------------------------------------------------------------ 4.82- 0.58 4510 333701.50 22.10 95.79 Scale applied to data: s=0.229019 (maximum obs:4366447.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.053; Rsigma 0.029: data 4510 -> merged 110 With outlier rejection... Rint 0.052; Rsigma 0.029: data 4497 -> merged 110 Rejected total: 13, method kkm 11, method Blessing 2 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585481, 4.828003 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 28.70 100.00 287 1.61 - 1.21 10 10 41.90 100.00 419 1.17 - 1.01 10 10 53.50 100.00 535 0.99 - 0.89 10 10 51.80 100.00 518 0.88 - 0.81 10 10 49.60 100.00 496 0.81 - 0.74 10 10 43.30 100.00 433 0.73 - 0.71 10 10 47.70 100.00 477 0.70 - 0.66 10 10 39.40 100.00 394 0.65 - 0.64 10 10 36.90 100.00 369 0.63 - 0.60 10 10 35.50 100.00 355 --------------------------------------------------------------- 8.36 - 0.60 100 100 42.83 100.00 4283 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:45:40 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.358073 8.365926 8.363044 89.9650 89.9950 89.9679 4499 Reflections read from file xs1714a.hkl; mean (I/sigma) = 21.99 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2295 0 3016 3020 4499 N (int>3sigma) = 0 0 0 0 2295 0 2894 2891 4312 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.2 77.8 75.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 22.0 22.1 22.0 Lattice type: F chosen Volume: 584.77 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.911 5.912 5.912 90.03 119.95 119.98 Niggli form: a.a = 34.942 b.b = 34.946 c.c = 34.953 b.c = -0.021 a.c = -17.445 a.b = -17.464 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.043 CUBIC F-lattice R(int) = 0.050 [ 4342] Vol = 584.8 Cell: 8.363 8.366 8.358 90.03 90.00 90.03 Volume: 584.77 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.042 RHOMBOHEDRAL R-lattice R(int) = 0.055 [ 4058] Vol = 438.6 Cell: 5.913 5.912 14.490 90.03 90.03 120.01 Volume: 438.58 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.042 RHOMBOHEDRAL R-lattice R(int) = 0.049 [ 1293] Vol = 438.6 Trigonal Cell: 5.913 5.912 14.490 90.03 90.03 120.01 Volume: 438.58 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.019 TETRAGONAL I-lattice R(int) = 0.049 [ 4092] Vol = 292.4 Cell: 5.916 5.913 8.358 89.98 89.97 89.98 Volume: 292.38 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.042 TETRAGONAL I-lattice R(int) = 0.049 [ 4092] Vol = 292.4 Cell: 5.913 5.916 8.358 90.03 90.02 89.98 Volume: 292.38 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4038] Vol = 292.4 Cell: 5.913 5.916 8.358 89.97 89.98 89.98 Volume: 292.38 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.027 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4034] Vol = 292.4 Cell: 5.911 8.363 5.914 89.97 89.95 89.98 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.013 MONOCLINIC I-lattice R(int) = 0.047 [ 3684] Vol = 292.4 Cell: 5.916 5.913 8.358 90.02 90.03 89.98 Volume: 292.38 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.032 MONOCLINIC I-lattice R(int) = 0.045 [ 3682] Vol = 292.4 Cell: 5.911 5.914 8.363 90.03 90.02 89.95 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.021 MONOCLINIC I-lattice R(int) = 0.045 [ 3697] Vol = 292.4 Cell: 5.911 8.363 5.914 89.97 90.05 90.02 Volume: 292.38 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.027 MONOCLINIC I-lattice R(int) = 0.045 [ 3680] Vol = 292.4 Cell: 5.914 5.911 8.363 89.98 90.03 90.05 Volume: 292.38 Matrix: 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.026 MONOCLINIC C-lattice R(int) = 0.045 [ 3681] Vol = 292.4 Cell: 10.240 5.912 5.912 90.03 125.22 89.98 Volume: 292.38 Matrix: 0.5000 -1.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.042 [ 3006] Vol = 146.2 Cell: 5.911 5.912 5.912 90.03 119.95 119.98 Volume: 146.19 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2295 0 3016 3029 4499 N (int>3sigma) = 0 0 0 0 2295 0 2894 2903 4312 Mean intensity = 0.0 0.0 0.0 0.0 30.1 0.0 76.2 76.2 75.9 Mean int/sigma = 0.0 0.0 0.0 0.0 22.8 0.0 22.0 22.1 22.0 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.160 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 47 47 345 1007 N I>3s 46 46 315 1007 0.9 0.9 0.7 35.9 8.5 8.5 5.1 25.5 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.050 4017 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4056 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.363044 8.365926 8.358073 90.0321 89.9950 90.0350 ZERR 3.00 0.000446 0.000521 0.000564 0.0053 0.0049 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3714276- 482958 999 994 27 36.8 1152779.81 38.56 0.049 0.062 465292- 112286 1327 1326 27 49.1 200128.97 29.19 0.056 0.070 99365- 33232 1114 1113 27 41.2 73244.59 15.89 0.073 0.094 9765- 1753 1070 1064 29 36.7 3280.67 4.35 0.175 0.235 ------------------------------------------------------------------------------------------- 3714276- 1753 4510 4497 110 40.9 332720.93 22.09 0.052 0.065 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1151 1145 27 42.4 599318.45 31.27 0.047 0.061 0.024 1.01-0.78 1378 1377 28 49.2 305800.11 21.33 0.045 0.056 0.029 0.76-0.65 1187 1185 28 42.3 229369.75 18.60 0.063 0.076 0.035 0.65-0.59 794 790 27 29.3 148274.01 15.36 0.079 0.085 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 4510 4497 110 40.9 332720.93 22.09 0.052 0.065 0.029 inf-0.60 4292 4281 99 43.2 344808.10 22.57 0.051 0.065 0.029 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1145 27 27 100.0 42.4 599318.45 227.87 0.047 0.005 1.01-0.78 1377 28 28 100.0 49.2 305800.11 159.21 0.045 0.004 0.76-0.65 1185 28 28 100.0 42.3 229369.75 128.80 0.063 0.006 0.65-0.59 790 27 27 100.0 29.3 148274.01 96.01 0.079 0.012 -------------------------------------------------------------------------------------------- inf-0.59 4497 110 110 100.0 40.9 332720.93 157.57 0.052 0.006 inf-0.60 4281 99 99 100.0 43.2 344808.10 161.98 0.051 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:51:54 2018) ID: 2932; threads 39; handles 878; mem 519364.00 (1237720.00)kB; time: 1w 5d 1h 57m 25s MEMORY INFO: Memory PF:0.0, Ph:234.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:507.2,peak PF: 697.1, WS: 297.4, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:0.0, Ph:234.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:509.0,peak PF: 697.1, WS: 299.2, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:51:54 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000005 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) 8.37024 ( 0.00057 ) 8.37691 ( 0.00052 ) 8.37554 ( 0.00045 ) 90.02113 ( 0.00475 ) 90.03240 ( 0.00495 ) 90.03043 ( 0.00526 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:51:55 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000005 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007202 -0.000004 -0.000001 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000001 -0.000004 0.007193 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(6) 8.3769(5) 8.3755(4) 90.021(5) 90.032(5) 90.030(5) V = 587.27(6) unit cell: 8.36235(17) 8.36235(17) 8.36235(17) 90.0 90.0 90.0 V = 584.77(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 452 peaks identified as outliers and rejected 445 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 445 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 445 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.983 ( 0.172) | 1.325 ( 0.738) | 1.574 ( 2.293) | 1.33- 1.09 | 45 | 1.069 ( 0.114) | 1.092 ( 0.140) | 1.111 ( 0.488) | 1.09- 0.94 | 45 | 1.053 ( 0.114) | 1.073 ( 0.140) | 1.090 ( 0.408) | 0.94- 0.84 | 45 | 1.079 ( 0.108) | 1.069 ( 0.142) | 1.120 ( 0.394) | 0.84- 0.78 | 45 | 1.107 ( 0.101) | 1.022 ( 0.128) | 1.379 ( 0.502) | 0.78- 0.73 | 45 | 1.107 ( 0.080) | 0.977 ( 0.111) | 1.379 ( 0.507) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.930 ( 0.103) | 1.364 ( 0.510) | 0.69- 0.65 | 45 | 1.069 ( 0.074) | 0.887 ( 0.098) | 1.320 ( 0.461) | 0.65- 0.62 | 45 | 1.049 ( 0.078) | 0.846 ( 0.047) | 1.390 ( 0.609) | 0.62- 0.59 | 40 | 1.021 ( 0.082) | 0.806 ( 0.034) | 1.400 ( 0.563) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 445 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.312 ( 0.881) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 444 obs out of 445 (total:445,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028945 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036035 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000025 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000025 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3857(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.803(12) V = 589.18(16) OTKP changes: 444 1 1 1 No constraint UB - matrix: -0.024649 -0.079495 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028812 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036126 -0.003521 0.076557 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079495 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028812 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036126 -0.003521 0.076557 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) unit cell: 8.3743(12) 8.3813(11) 8.3654(12) 90.042(11) 90.078(12) 89.974(11) V = 587.15(14) unit cell: 8.3737(4) 8.3737(4) 8.3737(4) 90.0 90.0 90.0 V = 587.15(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.912) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079495 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028812 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036126 -0.003521 0.076557 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079495 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028812 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036126 -0.003521 0.076557 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) unit cell: 8.3743(12) 8.3813(11) 8.3654(12) 90.042(11) 90.078(12) 89.974(11) V = 587.15(14) unit cell: 8.3737(4) 8.3737(4) 8.3737(4) 90.0 90.0 90.0 V = 587.15(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 445 obs out of 445 (total:445,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 448 peaks identified as outliers and rejected 440 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 440 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 440 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.986 ( 0.169) | 1.298 ( 0.707) | 1.555 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.087 ( 0.140) | 1.155 ( 0.505) | 1.09- 0.96 | 44 | 1.063 ( 0.105) | 1.084 ( 0.143) | 1.117 ( 0.479) | 0.96- 0.84 | 44 | 1.073 ( 0.111) | 1.056 ( 0.136) | 1.145 ( 0.403) | 0.84- 0.81 | 44 | 1.112 ( 0.099) | 1.034 ( 0.130) | 1.356 ( 0.480) | 0.81- 0.73 | 44 | 1.088 ( 0.089) | 0.989 ( 0.129) | 1.292 ( 0.473) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.949 ( 0.114) | 1.391 ( 0.482) | 0.70- 0.67 | 44 | 1.077 ( 0.072) | 0.883 ( 0.071) | 1.433 ( 0.477) | 0.67- 0.63 | 44 | 1.073 ( 0.063) | 0.870 ( 0.063) | 1.463 ( 0.597) | 0.63- 0.59 | 44 | 1.011 ( 0.080) | 0.807 ( 0.036) | 1.267 ( 0.484) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 440 | 1.064 ( 0.108) | 1.006 ( 0.282) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 39 | 1.034 ( 0.140) | 1.212 ( 0.488) | 1.144 ( 0.710) | 1.41- 1.17 | 39 | 1.017 ( 0.109) | 1.175 ( 0.516) | 1.084 ( 0.530) | 1.17- 0.99 | 39 | 1.025 ( 0.094) | 1.047 ( 0.109) | 0.944 ( 0.361) | 0.99- 0.89 | 39 | 1.018 ( 0.096) | 1.012 ( 0.121) | 1.026 ( 0.379) | 0.89- 0.82 | 39 | 1.019 ( 0.086) | 1.008 ( 0.096) | 1.145 ( 0.483) | 0.82- 0.75 | 39 | 1.007 ( 0.087) | 0.964 ( 0.126) | 1.064 ( 0.402) | 0.75- 0.71 | 39 | 0.968 ( 0.066) | 0.899 ( 0.082) | 1.221 ( 0.547) | 0.71- 0.67 | 39 | 0.965 ( 0.044) | 0.877 ( 0.053) | 1.246 ( 0.535) | 0.67- 0.63 | 39 | 0.948 ( 0.039) | 0.830 ( 0.043) | 1.280 ( 0.452) | 0.63- 0.59 | 43 | 0.909 ( 0.040) | 0.782 ( 0.038) | 1.129 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 394 | 0.990 ( 0.094) | 0.978 ( 0.273) | 1.128 ( 0.501) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 8 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb PROFFITPEAK info: 881 peaks in the peak location table UB fit with 390 obs out of 432 (total:432,skipped:0) (90.28%) UB - matrix: -0.025353 -0.079297 -0.015630 ( 0.000039 0.000027 0.000046 ) 0.072420 -0.029475 0.032810 ( 0.000033 0.000023 0.000040 ) -0.036235 -0.003711 0.076529 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007200 0.000010 -0.000001 ( 0.000006 0.000004 0.000004 ) 0.000010 0.007171 -0.000012 ( 0.000004 0.000004 0.000004 ) -0.000001 -0.000012 0.007178 ( 0.000004 0.000004 0.000007 ) unit cell: 8.359(3) 8.376(3) 8.372(4) 89.91(3) 89.99(3) 90.08(3) V = 586.2(4) UB fit with 390 obs out of 432 (total:432,skipped:0) (90.28%) UB - matrix: -0.025353 -0.079297 -0.015630 ( 0.000039 0.000027 0.000046 ) 0.072420 -0.029475 0.032810 ( 0.000033 0.000023 0.000040 ) -0.036235 -0.003711 0.076529 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007200 0.000010 -0.000001 ( 0.000006 0.000004 0.000004 ) 0.000010 0.007171 -0.000012 ( 0.000004 0.000004 0.000004 ) -0.000001 -0.000012 0.007178 ( 0.000004 0.000004 0.000007 ) unit cell: 8.359(3) 8.376(3) 8.372(4) 89.91(3) 89.99(3) 90.08(3) V = 586.2(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.025386 -0.079266 -0.015656 ( 0.000037 0.000026 0.000044 ) 0.072393 -0.029534 0.032836 ( 0.000034 0.000024 0.000040 ) -0.036292 -0.003662 0.076499 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007202 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007169 -0.000009 ( 0.000004 0.000004 0.000004 ) -0.000002 -0.000009 0.007175 ( 0.000004 0.000004 0.000007 ) UB fit with 393 obs out of 432 (total:432,skipped:0) (90.97%) unit cell: 8.358(3) 8.377(3) 8.373(4) 89.93(3) 89.99(3) 90.06(3) V = 586.3(4) UB fit with 393 obs out of 432 (total:432,skipped:0) (90.97%) UB - matrix: -0.025386 -0.079266 -0.015656 ( 0.000037 0.000026 0.000044 ) 0.072393 -0.029534 0.032836 ( 0.000034 0.000024 0.000040 ) -0.036292 -0.003662 0.076499 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007202 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007169 -0.000009 ( 0.000004 0.000004 0.000004 ) -0.000002 -0.000009 0.007175 ( 0.000004 0.000004 0.000007 ) unit cell: 8.358(3) 8.377(3) 8.373(4) 89.93(3) 89.99(3) 90.06(3) V = 586.3(4) OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 OTKP changes: 75 1 1 1 UB - matrix: -0.025386 -0.079266 -0.015656 ( 0.000037 0.000026 0.000044 ) 0.072393 -0.029534 0.032836 ( 0.000034 0.000024 0.000040 ) -0.036292 -0.003662 0.076499 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007202 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007169 -0.000009 ( 0.000004 0.000004 0.000004 ) -0.000002 -0.000009 0.007175 ( 0.000004 0.000004 0.000007 ) UB fit with 393 obs out of 432 (total:432,skipped:0) (90.97%) unit cell: 8.358(3) 8.377(3) 8.373(4) 89.93(3) 89.99(3) 90.06(3) V = 586.3(4) 432 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Run 8 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 593 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025386 -0.079266 -0.015656 ( 0.000037 0.000026 0.000044 ) 0.072393 -0.029534 0.032836 ( 0.000034 0.000024 0.000040 ) -0.036292 -0.003662 0.076499 ( 0.000033 0.000023 0.000040 ) M - matrix: 0.007202 0.000007 -0.000002 ( 0.000006 0.000004 0.000004 ) 0.000007 0.007169 -0.000009 ( 0.000004 0.000004 0.000004 ) -0.000002 -0.000009 0.007175 ( 0.000004 0.000004 0.000007 ) UB fit with 393 obs out of 432 (total:432,skipped:0) (90.97%) unit cell: 8.358(3) 8.377(3) 8.373(4) 89.93(3) 89.99(3) 90.06(3) V = 586.3(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 392 obs out of 432 (total:432,skipped:0) (90.74%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb 5 of 332 peaks identified as outliers and rejected 327 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 327 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 327 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 33 | 1.064 ( 0.146) | 1.247 ( 0.593) | 1.173 ( 0.652) | 1.41- 1.17 | 33 | 1.069 ( 0.127) | 1.166 ( 0.447) | 1.095 ( 0.470) | 1.15- 1.01 | 33 | 1.026 ( 0.102) | 1.017 ( 0.114) | 1.135 ( 0.533) | 0.98- 0.91 | 33 | 1.037 ( 0.086) | 1.006 ( 0.124) | 1.157 ( 0.419) | 0.91- 0.82 | 33 | 1.036 ( 0.082) | 1.013 ( 0.123) | 1.048 ( 0.465) | 0.82- 0.75 | 33 | 1.028 ( 0.059) | 0.983 ( 0.097) | 1.302 ( 0.549) | 0.75- 0.71 | 33 | 0.999 ( 0.051) | 0.931 ( 0.081) | 1.164 ( 0.411) | 0.71- 0.67 | 33 | 0.966 ( 0.038) | 0.899 ( 0.052) | 1.141 ( 0.475) | 0.67- 0.62 | 33 | 0.938 ( 0.046) | 0.864 ( 0.048) | 1.408 ( 0.574) | 0.62- 0.59 | 30 | 0.898 ( 0.048) | 0.830 ( 0.038) | 1.255 ( 0.580) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 327 | 1.007 ( 0.101) | 0.997 ( 0.278) | 1.187 ( 0.527) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 325 obs out of 327 (total:327,skipped:0) (99.39%) UB - matrix: -0.025361 -0.079427 -0.015643 ( 0.000018 0.000013 0.000020 ) 0.072379 -0.029491 0.032866 ( 0.000015 0.000010 0.000017 ) -0.036131 -0.003710 0.076666 ( 0.000021 0.000014 0.000022 ) M - matrix: 0.007187 0.000014 0.000005 ( 0.000003 0.000002 0.000002 ) 0.000014 0.007192 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000005 -0.000011 0.007203 ( 0.000002 0.000002 0.000004 ) unit cell: 8.3666(16) 8.3638(14) 8.358(2) 89.910(16) 90.044(18) 90.111(15) V = 584.8(2) OTKP changes: 325 1 1 1 OTKP changes: 325 1 1 1 OTKP changes: 325 1 1 1 No constraint UB - matrix: -0.025311 -0.079307 -0.015704 ( 0.000019 0.000013 0.000020 ) 0.072317 -0.029566 0.032857 ( 0.000016 0.000011 0.000017 ) -0.036260 -0.003629 0.076530 ( 0.000016 0.000011 0.000017 ) M - matrix: 0.007185 0.000001 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000001 0.007177 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000004 0.007183 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.025311 -0.079307 -0.015704 ( 0.000019 0.000013 0.000020 ) 0.072317 -0.029566 0.032857 ( 0.000016 0.000011 0.000017 ) -0.036260 -0.003629 0.076530 ( 0.000016 0.000011 0.000017 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 326 obs out of 327 (total:327,skipped:0) (99.69%) unit cell: 8.3678(16) 8.3726(14) 8.3690(17) 89.970(15) 89.989(16) 90.006(15) V = 586.34(19) unit cell: 8.3698(4) 8.3698(4) 8.3698(4) 90.0 90.0 90.0 V = 586.34(5) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 594 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025311 -0.079307 -0.015704 ( 0.000019 0.000013 0.000020 ) 0.072317 -0.029566 0.032857 ( 0.000016 0.000011 0.000017 ) -0.036260 -0.003629 0.076530 ( 0.000016 0.000011 0.000017 ) M - matrix: 0.007185 0.000001 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000001 0.007177 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000004 0.007183 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.025311 -0.079307 -0.015704 ( 0.000019 0.000013 0.000020 ) 0.072317 -0.029566 0.032857 ( 0.000016 0.000011 0.000017 ) -0.036260 -0.003629 0.076530 ( 0.000016 0.000011 0.000017 ) M - matrix: 0.007181 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007181 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007181 ( 0.000000 0.000000 0.000001 ) UB fit with 326 obs out of 327 (total:327,skipped:0) (99.69%) unit cell: 8.3678(16) 8.3726(14) 8.3690(17) 89.970(15) 89.989(16) 90.006(15) V = 586.34(19) unit cell: 8.3698(4) 8.3698(4) 8.3698(4) 90.0 90.0 90.0 V = 586.34(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 326 obs out of 327 (total:327,skipped:0) (99.69%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb 5 of 330 peaks identified as outliers and rejected 325 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 325 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 325 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 33 | 1.045 ( 0.111) | 1.238 ( 0.585) | 1.160 ( 0.565) | 1.41- 1.17 | 33 | 1.070 ( 0.128) | 1.131 ( 0.399) | 1.068 ( 0.441) | 1.15- 0.98 | 33 | 1.035 ( 0.101) | 1.033 ( 0.114) | 1.100 ( 0.508) | 0.98- 0.89 | 33 | 1.029 ( 0.088) | 0.990 ( 0.120) | 1.173 ( 0.442) | 0.89- 0.82 | 33 | 1.045 ( 0.076) | 1.016 ( 0.114) | 1.159 ( 0.553) | 0.82- 0.75 | 33 | 1.020 ( 0.056) | 0.983 ( 0.091) | 1.208 ( 0.492) | 0.75- 0.71 | 33 | 0.993 ( 0.050) | 0.925 ( 0.080) | 1.109 ( 0.417) | 0.71- 0.67 | 33 | 0.965 ( 0.040) | 0.895 ( 0.051) | 1.193 ( 0.483) | 0.67- 0.62 | 33 | 0.936 ( 0.048) | 0.864 ( 0.050) | 1.349 ( 0.603) | 0.62- 0.59 | 28 | 0.904 ( 0.045) | 0.835 ( 0.036) | 1.298 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 325 | 1.006 ( 0.094) | 0.993 ( 0.266) | 1.180 ( 0.516) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.8 | 344 | 1.117 ( 0.116) | 1.236 ( 0.464) | 1.234 ( 0.994) | 12.8-18.5 | 344 | 1.078 ( 0.050) | 1.120 ( 0.231) | 1.175 ( 0.496) | 18.5-22.8 | 344 | 1.065 ( 0.070) | 1.127 ( 0.347) | 1.181 ( 0.548) | 22.8-27.1 | 344 | 1.033 ( 0.082) | 1.077 ( 0.287) | 1.136 ( 0.552) | 27.1-30.5 | 344 | 1.005 ( 0.069) | 1.010 ( 0.275) | 1.184 ( 0.488) | 30.5-33.6 | 344 | 0.974 ( 0.073) | 0.926 ( 0.090) | 1.176 ( 0.514) | 33.6-36.8 | 344 | 0.952 ( 0.067) | 0.905 ( 0.118) | 1.141 ( 0.468) | 36.8-39.6 | 344 | 0.935 ( 0.077) | 0.868 ( 0.116) | 1.200 ( 0.536) | 39.6-42.6 | 344 | 0.918 ( 0.069) | 0.841 ( 0.110) | 1.182 ( 0.541) | 42.6-50.7 | 346 | 0.918 ( 0.081) | 0.809 ( 0.064) | 1.164 ( 0.491) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3442 | 0.999 ( 0.103) | 0.992 ( 0.280) | 1.177 ( 0.582) | Fitted profile normalization line parameters e1 dimension: a=-0.0050 b=1.16 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0016 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708053 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 16:52:34 2018 PROFFITMAIN - Started at Tue Mar 27 16:52:34 2018 OTKP changes: 3432 2 4 6 OTKP changes: 3432 2 4 6 OTKP changes: 3432 2 4 6 No constraint UB - matrix: -0.025069 -0.079495 -0.015622 ( 0.000005 0.000005 0.000005 ) 0.072526 -0.029316 0.032934 ( 0.000005 0.000005 0.000005 ) -0.036241 -0.003610 0.076608 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007202 -0.000002 0.000004 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007192 -0.000000 ( 0.000001 0.000001 0.000001 ) 0.000004 -0.000000 0.007197 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025069 -0.079495 -0.015622 ( 0.000005 0.000005 0.000005 ) 0.072526 -0.029316 0.032934 ( 0.000005 0.000005 0.000005 ) -0.036241 -0.003610 0.076608 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000000 ) UB fit with 3437 obs out of 3442 (total:3442,skipped:0) (99.85%) unit cell: 8.3581(5) 8.3639(5) 8.3607(4) 89.999(4) 90.031(4) 89.980(5) V = 584.47(6) unit cell: 8.36090(13) 8.36090(13) 8.36090(13) 90.0 90.0 90.0 V = 584.466(15) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) UB - matrix: -0.024720 -0.079528 -0.015416 ( 0.000014 0.000011 0.000013 ) 0.072528 -0.028880 0.033050 ( 0.000012 0.000010 0.000012 ) -0.036074 -0.003519 0.076553 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007173 -0.000002 0.000017 ( 0.000002 0.000001 0.000001 ) -0.000002 0.007171 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000017 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3751(12) 8.3760(12) 8.3648(12) 90.017(11) 90.133(11) 89.986(11) V = 586.79(14) OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 OTKP changes: 439 1 1 1 No constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.050(11) 90.081(11) 89.972(11) V = 583.49(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.49(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.717) HKL list info: 805 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.050(11) 90.081(11) 89.972(11) V = 583.49(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.49(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007204 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024712 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072659 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036256 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 440 obs out of 440 (total:440,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.050(11) 90.081(11) 89.972(11) V = 583.49(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.49(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024855 -0.079562 -0.015643 ( 0.000013 0.000015 0.000011 ) 0.072446 -0.029185 0.032940 ( 0.000016 0.000018 0.000013 ) -0.036281 -0.003656 0.076382 ( 0.000011 0.000012 0.000009 ) M - matrix: 0.007183 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007195 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3693(14) 8.3619(14) 8.3802(10) 90.032(12) 90.031(12) 89.966(14) V = 586.48(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024996 -0.079537 -0.015503 ( 0.000017 0.000014 0.000012 ) 0.072494 -0.029266 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036257 -0.003618 0.076526 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007196 -0.000010 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000010 0.007186 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3622(11) 8.3617(14) 8.3675(11) 89.924(12) 90.042(11) 89.981(12) V = 585.07(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.15(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.15(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.717) HKL list info: 784 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.15(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.15(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.15(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.15(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025030 -0.079530 -0.015725 ( 0.000008 0.000013 0.000012 ) 0.072415 -0.029343 0.032923 ( 0.000008 0.000014 0.000014 ) -0.036208 -0.003658 0.076531 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007199 0.000005 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000005 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3700(11) 8.3595(12) 8.3661(11) 90.037(11) 90.054(11) 89.985(11) V = 585.37(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.717) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025243 -0.079452 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072370 -0.029419 0.032789 ( 0.000008 0.000011 0.000012 ) -0.036254 -0.003623 0.076603 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007189 0.000008 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000006 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3656(10) 8.3643(14) 8.3642(11) 90.078(12) 89.948(10) 90.063(12) V = 585.26(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3570(14) 8.3523(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.717) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3570(14) 8.3523(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3570(14) 8.3523(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025308 -0.079442 -0.015638 ( 0.000010 0.000008 0.000010 ) 0.072447 -0.029451 0.032791 ( 0.000014 0.000011 0.000014 ) -0.036122 -0.003538 0.076589 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000005 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000005 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007186 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3628(13) 8.3645(9) 8.3675(12) 90.045(10) 90.038(12) 90.037(10) V = 585.31(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.068(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.717) HKL list info: 791 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.068(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.068(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb Run 7 has been already processed *** 3D integration started - run 8 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 325 obs out of 325 (total:325,skipped:0) (100.00%) UB - matrix: -0.025341 -0.079343 -0.015679 ( 0.000019 0.000013 0.000020 ) 0.072350 -0.029514 0.032819 ( 0.000016 0.000011 0.000017 ) -0.036183 -0.003688 0.076586 ( 0.000016 0.000011 0.000017 ) M - matrix: 0.007186 0.000009 0.000001 ( 0.000003 0.000002 0.000002 ) 0.000009 0.007180 -0.000007 ( 0.000002 0.000002 0.000002 ) 0.000001 -0.000007 0.007188 ( 0.000002 0.000002 0.000003 ) unit cell: 8.3674(16) 8.3708(14) 8.3660(16) 89.944(15) 90.005(16) 90.070(15) V = 585.97(19) OTKP changes: 325 1 1 1 OTKP changes: 325 1 1 1 OTKP changes: 325 1 1 1 No constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007205 0.000002 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000002 0.007194 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000004 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 325 obs out of 325 (total:325,skipped:0) (100.00%) unit cell: 8.3561(16) 8.3626(14) 8.3580(16) 89.972(15) 89.990(15) 90.016(15) V = 584.05(18) unit cell: 8.3589(3) 8.3589(3) 8.3589(3) 90.0 90.0 90.0 V = 584.05(4) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.717) HKL list info: 588 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007205 0.000002 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000002 0.007194 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000004 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 325 obs out of 325 (total:325,skipped:0) (100.00%) unit cell: 8.3561(16) 8.3626(14) 8.3580(16) 89.972(15) 89.990(15) 90.016(15) V = 584.05(18) unit cell: 8.3589(3) 8.3589(3) 8.3589(3) 90.0 90.0 90.0 V = 584.05(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 325 obs out of 325 (total:325,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007205 0.000002 -0.000001 ( 0.000003 0.000002 0.000002 ) 0.000002 0.007194 -0.000004 ( 0.000002 0.000002 0.000002 ) -0.000001 -0.000004 0.007202 ( 0.000002 0.000002 0.000003 ) Constraint UB - matrix: -0.025328 -0.079424 -0.015665 ( 0.000019 0.000013 0.000020 ) 0.072434 -0.029546 0.032904 ( 0.000017 0.000011 0.000018 ) -0.036291 -0.003595 0.076642 ( 0.000015 0.000010 0.000016 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 325 obs out of 325 (total:325,skipped:0) (100.00%) unit cell: 8.3561(16) 8.3626(14) 8.3580(16) 89.972(15) 89.990(15) 90.016(15) V = 584.05(18) unit cell: 8.3589(3) 8.3589(3) 8.3589(3) 90.0 90.0 90.0 V = 584.05(4) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=75, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025067 -0.079460 -0.015598 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029340 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036260 -0.003631 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007203 -0.000004 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 -0.000004 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025067 -0.079460 -0.015598 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029340 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036260 -0.003631 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) UB fit with 3437 obs out of 3442 (total:3442,skipped:0) (99.85%) unit cell: 8.3576(5) 8.3662(5) 8.3626(4) 89.966(5) 90.000(5) 89.966(5) V = 584.73(6) unit cell: 8.36215(16) 8.36215(16) 8.36215(16) 90.0 90.0 90.0 V = 584.73(2) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 79 reflections under beam stop or inside a detector rejection region 26 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_8.rrpprof 4654 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 16:52:43 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.717) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.717) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.717) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.717) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.717) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.717) PROFFIT INFO: signal sum: min=119.0000 max=23034060.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3186289.0181 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=559 PROFFIT INFO: Inet: min=293.3857 max=5098062.5000 PROFFIT INFO: sig(Inet): min=120.1888 max=47819.6250 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.06 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 63 256 523 958 1081 1994 3151 4287 4654 Percent 0.0 0.0 1.4 5.5 11.2 20.6 23.2 42.8 67.7 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4654 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4654 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5098063- 1076036 465 1796564.88 121.46 100.00 1071057- 581203 465 801708.88 100.05 100.00 580576- 246199 465 383615.42 92.46 100.00 245819- 159964 465 192782.07 69.54 100.00 159890- 113016 465 135023.03 48.88 100.00 112972- 85979 465 98922.32 35.08 100.00 85977- 58799 465 73166.78 27.59 100.00 58671- 5062 465 32315.02 17.76 100.00 5052- 2742 465 3614.89 5.16 94.84 2737- 293 469 1947.54 3.59 50.53 ------------------------------------------------------------------------------------ 5098063- 293 4654 351665.25 52.11 94.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 736419.42 90.69 100.00 1.41- 1.12 465 546111.82 65.55 99.35 1.12- 0.96 465 511002.85 68.23 96.56 0.96- 0.87 465 328653.72 58.16 93.12 0.87- 0.81 465 428560.13 67.16 99.35 0.81- 0.73 465 230900.35 40.05 95.48 0.73- 0.71 465 168010.60 33.84 89.46 0.71- 0.65 465 288890.93 45.15 92.47 0.65- 0.62 465 143193.51 26.37 86.02 0.62- 0.58 469 136757.84 26.18 93.18 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 351665.25 52.11 94.50 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:52:44 2018 Sorting 4654 observations 119 unique observations with > 7.00 F2/sig(F2) 4654 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 74 793 Total number of frames 793 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4654 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 10 118 Total number of frames 118 3726 observations > 7.00 F2/sig(F2) 3726 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 10 118 Total number of frames 118 Removing 'redundancy=1' reflections Average redundancy: 28.6 (Out of 3726 removed 4 = 3722, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3722 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 10 118 Total number of frames 118 130 unique data precomputed (should be 130) 130 unique data with 3722 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 28.6 (Out of 3722 removed 0 = 3722, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3722 observations RMS deviation of equivalent data = 0.25856 Rint = 0.20088 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19667, wR= 0.27196 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15733, wR= 0.20602, Acormin=0.599, Acormax=1.319, Acor_av=0.992 F test: Probability=1.000, F= 1.560 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13229, wR= 0.17216, Acormin=0.566, Acormax=1.406, Acor_av=0.956 F test: Probability=1.000, F= 1.413 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13547, wR= 0.18157, Acormin=0.591, Acormax=1.527, Acor_av=0.970 F test: Probability=0.000, F= 0.952 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10779, wR= 0.14632, Acormin=0.518, Acormax=1.534, Acor_av=0.944 F test: Probability=1.000, F= 1.502 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10008, wR= 0.13490, Acormin=0.445, Acormax=1.563, Acor_av=0.945 F test: Probability=1.000, F= 1.158 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12604, wR= 0.16899, Acormin=0.598, Acormax=1.600, Acor_av=0.972 F test: Probability=0.000, F= 0.630 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09964, wR= 0.13576, Acormin=0.519, Acormax=1.646, Acor_av=0.942 F test: Probability=0.585, F= 1.007 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09206, wR= 0.12561, Acormin=0.466, Acormax=1.648, Acor_av=0.947 F test: Probability=1.000, F= 1.178 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08915, wR= 0.11946, Acormin=0.336, Acormax=1.518, Acor_av=0.879 F test: Probability=0.966, F= 1.063 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11729, wR= 0.15249, Acormin=0.441, Acormax=1.447, Acor_av=0.843 F test: Probability=0.000, F= 0.578 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10111, wR= 0.13396, Acormin=0.493, Acormax=1.573, Acor_av=0.898 F test: Probability=0.000, F= 0.778 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10131, wR= 0.13102, Acormin=0.069, Acormax=0.317, Acor_av=0.174 F test: Probability=0.000, F= 0.773 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09313, wR= 0.12217, Acormin=0.066, Acormax=0.344, Acor_av=0.189 F test: Probability=0.000, F= 0.912 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08464, wR= 0.11299, Acormin=0.071, Acormax=0.364, Acor_av=0.199 F test: Probability=0.998, F= 1.099 Final absorption model (ne=6, no=5): Rint= 0.08915, Acormin=0.336, Acormax=1.518, Acor_av=0.879 Combined refinement in use Rint: 0.20100 There are 118 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 165 pars with 13695 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25856 Using Levenberg-Marquardt: 0.00010 New wR= 0.07127 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20088 with corrections 0.05671 Rint for all data: 0.20100 with corrections 0.05693 3 observations identified as outliers and rejected Cycle 2 wR= 0.07118 Using Levenberg-Marquardt: 0.00001 New wR= 0.06523 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19994 with corrections 0.05124 Rint for all data: 0.20100 with corrections 0.05158 0 observations identified as outliers and rejected Cycle 3 wR= 0.06523 Using Levenberg-Marquardt: 0.00000 New wR= 0.06343 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19994 with corrections 0.04990 Rint for all data: 0.20100 with corrections 0.05023 0 observations identified as outliers and rejected Cycle 4 wR= 0.06343 Using Levenberg-Marquardt: 0.00000 New wR= 0.06248 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19994 with corrections 0.04917 Rint for all data: 0.20100 with corrections 0.04949 0 observations identified as outliers and rejected Cycle 5 wR= 0.06248 Using Levenberg-Marquardt: 0.00000 New wR= 0.06194 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.19994 with corrections 0.04873 Rint for all data: 0.20100 with corrections 0.04904 0 observations identified as outliers and rejected Final wR= 0.06194 Final frame scales: Min= 0.7018 Max= 1.2293 Final absorption correction factors: Amin= 0.4725 Amax= 1.4609 PROFFIT INFO: Inet (after scale3 abspack): min=598.8854 max=4287355.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=135.1108 max=53430.9453 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4654 reflections read from tmp file 1032 reflections are rejected (1032 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 1 3 4 2 5 3 2 133 Initial Chi^2= 0.44140 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.84452 Current error model SIG(F2)^2 = 131.28*I_RAW + 0.00*I_BACK+(0.02577*)^2 Cycle 2, Chi^2= 1.00055 Current error model SIG(F2)^2 = 120.55*I_RAW + 0.00*I_BACK+(0.02137*)^2 Cycle 3, Chi^2= 0.99998 Current error model SIG(F2)^2 = 119.62*I_RAW + 0.00*I_BACK+(0.02159*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 119.76*I_RAW + 0.00*I_BACK+(0.02156*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 119.76*I_RAW + 0.00*I_BACK+(0.02156*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4287356- 1035402 465 1678743.35 43.16 100.00 1035321- 561686 465 760427.44 36.17 100.00 560539- 239658 465 373676.65 34.83 100.00 239637- 144557 465 180006.04 30.36 100.00 144284- 115923 465 130201.51 24.43 100.00 115742- 81438 465 94396.21 18.70 100.00 81360- 62326 465 71908.86 15.93 100.00 62290- 4535 465 34843.75 11.19 100.00 4524- 2568 465 3358.39 4.42 93.55 2560- 599 469 1979.02 3.60 66.52 ------------------------------------------------------------------------------------ 4287356- 599 4654 332669.66 22.26 95.98 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 727351.18 35.12 100.00 1.41- 1.12 465 535209.90 27.49 99.57 1.12- 0.96 465 456648.40 26.75 97.20 0.96- 0.87 465 308875.34 22.85 94.62 0.87- 0.81 465 402691.99 26.32 99.35 0.81- 0.73 465 209963.62 18.20 96.56 0.73- 0.71 465 159852.00 16.99 91.18 0.71- 0.65 465 268970.53 21.02 96.34 0.65- 0.62 465 134423.26 13.86 90.32 0.62- 0.58 469 124501.05 14.09 94.67 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 332669.66 22.26 95.98 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 727351.18 35.12 100.00 4.82- 1.12 930 631280.54 31.31 99.78 4.82- 0.96 1395 573069.83 29.79 98.92 4.82- 0.87 1860 507021.20 28.05 97.85 4.82- 0.81 2325 486155.36 27.71 98.15 4.82- 0.73 2790 440123.40 26.12 97.89 4.82- 0.71 3255 400084.63 24.82 96.93 4.82- 0.65 3720 383695.37 24.34 96.85 4.82- 0.62 4185 355998.47 23.18 96.13 4.82- 0.58 4654 332669.66 22.26 95.98 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 332669.66 22.26 95.98 Scale applied to data: s=0.233244 (maximum obs:4287355.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.049; Rsigma 0.029: data 4654 -> merged 157 With outlier rejection... Rint 0.049; Rsigma 0.029: data 4645 -> merged 157 Rejected total: 9, method kkm 7, method Blessing 2 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585468, 4.827892 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 27.86 100.00 390 1.41 - 1.12 14 14 38.29 100.00 536 1.12 - 0.97 14 14 38.14 100.00 534 0.96 - 0.84 14 14 40.93 100.00 573 0.84 - 0.78 14 14 30.71 100.00 430 0.78 - 0.73 14 14 32.79 100.00 459 0.73 - 0.69 14 14 30.36 100.00 425 0.69 - 0.65 14 14 25.93 100.00 363 0.65 - 0.63 14 14 27.21 100.00 381 0.63 - 0.60 14 14 24.07 100.00 337 --------------------------------------------------------------- 8.36 - 0.60 140 140 31.63 100.00 4428 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:52:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.357626 8.366248 8.362591 89.9665 89.9999 89.9657 4645 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2368 0 3115 3119 4645 N (int>3sigma) = 0 0 0 0 2368 0 2994 2987 4458 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.0 79.4 77.6 Mean int/sigma = 0.0 0.0 0.0 0.0 23.0 0.0 22.3 22.4 22.3 Lattice type: F chosen Volume: 584.73 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.911 5.911 5.911 90.03 119.94 119.98 Niggli form: a.a = 34.940 b.b = 34.946 c.c = 34.946 b.c = -0.021 a.c = -17.442 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.050 CUBIC F-lattice R(int) = 0.049 [ 4488] Vol = 584.7 Cell: 8.363 8.366 8.358 90.03 90.00 90.03 Volume: 584.73 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.048 RHOMBOHEDRAL R-lattice R(int) = 0.054 [ 4204] Vol = 438.5 Cell: 5.913 5.911 14.489 90.03 90.03 120.01 Volume: 438.55 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.048 RHOMBOHEDRAL R-lattice R(int) = 0.048 [ 1342] Vol = 438.5 Trigonal Cell: 5.913 5.911 14.489 90.03 90.03 120.01 Volume: 438.55 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.020 TETRAGONAL I-lattice R(int) = 0.048 [ 4238] Vol = 292.4 Cell: 5.916 5.913 8.358 89.98 89.98 89.97 Volume: 292.36 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.042 TETRAGONAL I-lattice R(int) = 0.048 [ 4238] Vol = 292.4 Cell: 5.913 5.916 8.358 90.02 90.02 89.97 Volume: 292.36 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4184] Vol = 292.4 Cell: 5.913 5.916 8.358 89.98 89.98 89.97 Volume: 292.36 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4180] Vol = 292.4 Cell: 5.911 8.363 5.915 89.98 89.94 89.98 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.016 MONOCLINIC I-lattice R(int) = 0.046 [ 3830] Vol = 292.4 Cell: 5.916 5.913 8.358 90.02 90.02 89.97 Volume: 292.36 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.036 MONOCLINIC I-lattice R(int) = 0.045 [ 3828] Vol = 292.4 Cell: 5.911 5.915 8.363 90.02 90.02 89.94 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.020 MONOCLINIC I-lattice R(int) = 0.044 [ 3843] Vol = 292.4 Cell: 5.911 8.363 5.915 89.98 90.06 90.02 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.029 MONOCLINIC I-lattice R(int) = 0.045 [ 3827] Vol = 292.4 Cell: 5.915 5.911 8.363 89.98 90.02 90.06 Volume: 292.36 Matrix: 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.027 MONOCLINIC C-lattice R(int) = 0.045 [ 3827] Vol = 292.4 Cell: 10.240 5.911 5.911 90.03 125.21 89.98 Volume: 292.36 Matrix: 0.5000 -1.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 3152] Vol = 146.2 Cell: 5.911 5.911 5.911 90.03 119.94 119.98 Volume: 146.18 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2368 0 3115 3126 4645 N (int>3sigma) = 0 0 0 0 2368 0 2994 3003 4458 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.0 78.5 77.6 Mean int/sigma = 0.0 0.0 0.0 0.0 23.0 0.0 22.3 22.4 22.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.162 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 50 50 355 1042 N I>3s 49 49 324 1042 1.0 1.0 0.7 36.6 8.6 8.6 5.2 25.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.049 4153 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4192 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362591 8.366248 8.357626 90.0343 89.9999 90.0335 ZERR 3.00 0.000435 0.000517 0.000553 0.0052 0.0048 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3720617- 690228 766 765 26 29.4 1345576.07 40.81 0.043 0.057 675640- 212968 708 705 26 27.1 416013.38 34.88 0.062 0.075 207392- 91717 1077 1077 26 41.4 139259.57 25.22 0.047 0.060 88044- 61657 762 762 26 29.3 75909.10 16.19 0.072 0.096 59845- 3174 617 615 26 23.7 21984.70 8.34 0.087 0.119 3128- 1695 724 721 27 26.7 2459.04 4.10 0.206 0.275 ------------------------------------------------------------------------------------------- 3720617- 1695 4654 4645 157 29.6 332782.34 22.26 0.049 0.064 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 878 874 26 33.6 583101.04 30.67 0.047 0.062 0.024 1.12-0.88 1031 1030 26 39.6 427959.23 25.83 0.038 0.050 0.027 0.85-0.75 857 857 26 33.0 306464.65 21.74 0.048 0.059 0.030 0.74-0.68 756 754 26 29.0 240141.35 19.48 0.058 0.070 0.035 0.67-0.63 712 712 26 27.4 136913.78 15.27 0.075 0.094 0.044 0.62-0.59 420 418 27 15.5 129560.45 13.84 0.078 0.077 0.045 ------------------------------------------------------------------------------------------------------ inf-0.59 4654 4645 157 29.6 332782.34 22.26 0.049 0.064 0.029 inf-0.60 4433 4426 139 31.8 344768.25 22.74 0.048 0.063 0.029 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 874 26 26 100.0 33.6 583101.04 193.10 0.047 0.005 1.12-0.88 1030 26 26 100.0 39.6 427959.23 165.58 0.038 0.005 0.85-0.75 857 26 26 100.0 33.0 306464.65 131.94 0.048 0.005 0.74-0.68 754 26 26 100.0 29.0 240141.35 107.37 0.058 0.007 0.67-0.63 712 26 26 100.0 27.4 136913.78 79.36 0.075 0.009 0.62-0.59 418 27 27 100.0 15.5 129560.45 62.58 0.078 0.016 -------------------------------------------------------------------------------------------- inf-0.59 4645 157 157 100.0 29.6 332782.34 132.62 0.049 0.006 inf-0.60 4426 139 139 100.0 31.8 344768.25 136.66 0.048 0.006 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025067 -0.079460 -0.015598 ( 0.000005 0.000005 0.000005 ) 0.072523 -0.029340 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036260 -0.003631 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007203 -0.000004 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 -0.000004 0.007194 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025067 -0.079460 -0.015598 ( 0.000005 0.000005 0.000005 ) 0.072523 -0.029340 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036260 -0.003631 0.076602 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007193 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007193 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007193 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3576(5) 8.3662(5) 8.3626(4) 89.966(5) 90.000(5) 89.966(5) V = 584.73(6) unit cell: 8.36215(16) 8.36215(16) 8.36215(16) 90.0 90.0 90.0 V = 584.73(2) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.717) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.717) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.717) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.717) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.717) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 34.000,75 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.717) PROFFIT INFO: signal sum: min=119.0000 max=23034060.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3186289.0181 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=553.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=559 PROFFIT INFO: Inet: min=293.3857 max=5098062.5000 PROFFIT INFO: sig(Inet): min=120.1888 max=47819.6250 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.06 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 126 512 1046 1916 2162 3988 6302 8574 9308 Percent 0.0 0.0 1.4 5.5 11.2 20.6 23.2 42.8 67.7 92.1 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4654 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4654 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5098063- 1076036 465 1796564.88 121.46 100.00 1071057- 581203 465 801708.88 100.05 100.00 580576- 246199 465 383615.42 92.46 100.00 245819- 159964 465 192782.07 69.54 100.00 159890- 113016 465 135023.03 48.88 100.00 112972- 85979 465 98922.32 35.08 100.00 85977- 58799 465 73166.78 27.59 100.00 58671- 5062 465 32315.02 17.76 100.00 5052- 2742 465 3614.89 5.16 94.84 2737- 293 469 1947.54 3.59 50.53 ------------------------------------------------------------------------------------ 5098063- 293 4654 351665.25 52.11 94.50 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 736419.42 90.69 100.00 1.41- 1.12 465 546111.82 65.55 99.35 1.12- 0.96 465 511002.85 68.23 96.56 0.96- 0.87 465 328653.72 58.16 93.12 0.87- 0.81 465 428560.13 67.16 99.35 0.81- 0.73 465 230900.35 40.05 95.48 0.73- 0.71 465 168010.60 33.84 89.46 0.71- 0.65 465 288890.93 45.15 92.47 0.65- 0.62 465 143193.51 26.37 86.02 0.62- 0.58 469 136757.84 26.18 93.18 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 351665.25 52.11 94.50 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 16:52:45 2018 Sorting 4654 observations 84 unique observations with > 7.00 F2/sig(F2) 4654 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 74 793 Total number of frames 793 Maximum number of 84 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4654 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 7 81 Total number of frames 81 3726 observations > 7.00 F2/sig(F2) 3726 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 7 81 Total number of frames 81 Removing 'redundancy=1' reflections Average redundancy: 40.0 (Out of 3726 removed 4 = 3722, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3722 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 7 81 Total number of frames 81 93 unique data precomputed (should be 93) 93 unique data with 3722 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 40.0 (Out of 3722 removed 0 = 3722, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3722 observations RMS deviation of equivalent data = 0.25915 Rint = 0.20115 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.19681, wR= 0.27223 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15761, wR= 0.20643, Acormin=0.599, Acormax=1.319, Acor_av=0.992 F test: Probability=1.000, F= 1.557 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13269, wR= 0.17247, Acormin=0.566, Acormax=1.408, Acor_av=0.956 F test: Probability=1.000, F= 1.410 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13563, wR= 0.18192, Acormin=0.592, Acormax=1.529, Acor_av=0.970 F test: Probability=0.000, F= 0.956 Trying model 4 (ne=4, no=1)... Results: Rint= 0.10785, wR= 0.14661, Acormin=0.516, Acormax=1.535, Acor_av=0.944 F test: Probability=1.000, F= 1.510 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10002, wR= 0.13538, Acormin=0.442, Acormax=1.566, Acor_av=0.946 F test: Probability=1.000, F= 1.160 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12600, wR= 0.16958, Acormin=0.599, Acormax=1.603, Acor_av=0.974 F test: Probability=0.000, F= 0.630 Trying model 7 (ne=6, no=1)... Results: Rint= 0.09971, wR= 0.13623, Acormin=0.516, Acormax=1.650, Acor_av=0.943 F test: Probability=0.554, F= 1.005 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09194, wR= 0.12623, Acormin=0.461, Acormax=1.654, Acor_av=0.949 F test: Probability=1.000, F= 1.179 Trying model 9 (ne=6, no=5)... Results: Rint= 0.08930, wR= 0.11993, Acormin=0.338, Acormax=1.522, Acor_av=0.880 F test: Probability=0.950, F= 1.057 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11725, wR= 0.15313, Acormin=0.449, Acormax=1.453, Acor_av=0.845 F test: Probability=0.000, F= 0.581 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10113, wR= 0.13448, Acormin=0.497, Acormax=1.578, Acor_av=0.899 F test: Probability=0.000, F= 0.780 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10151, wR= 0.13205, Acormin=0.069, Acormax=0.314, Acor_av=0.172 F test: Probability=0.000, F= 0.773 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09351, wR= 0.12316, Acormin=0.067, Acormax=0.341, Acor_av=0.187 F test: Probability=0.000, F= 0.908 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08508, wR= 0.11363, Acormin=0.070, Acormax=0.361, Acor_av=0.196 F test: Probability=0.996, F= 1.092 Final absorption model (ne=6, no=5): Rint= 0.08930, Acormin=0.338, Acormax=1.522, Acor_av=0.880 Combined refinement in use Rint: 0.20127 There are 81 active scales (one needs to be fixed) Refinement control: frame scale #58 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 128 pars with 8256 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25915 Using Levenberg-Marquardt: 0.00010 New wR= 0.07681 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20115 with corrections 0.06079 Rint for all data: 0.20127 with corrections 0.06101 2 observations identified as outliers and rejected Cycle 2 wR= 0.07659 Using Levenberg-Marquardt: 0.00001 New wR= 0.06994 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20026 with corrections 0.05463 Rint for all data: 0.20127 with corrections 0.05506 1 observations identified as outliers and rejected Cycle 3 wR= 0.06998 Using Levenberg-Marquardt: 0.00000 New wR= 0.06771 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20021 with corrections 0.05286 Rint for all data: 0.20127 with corrections 0.05329 0 observations identified as outliers and rejected Cycle 4 wR= 0.06771 Using Levenberg-Marquardt: 0.00000 New wR= 0.06636 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20021 with corrections 0.05189 Rint for all data: 0.20127 with corrections 0.05228 0 observations identified as outliers and rejected Cycle 5 wR= 0.06636 Using Levenberg-Marquardt: 0.00000 New wR= 0.06542 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20021 with corrections 0.05124 Rint for all data: 0.20127 with corrections 0.05162 0 observations identified as outliers and rejected Final wR= 0.06542 Final frame scales: Min= 0.7672 Max= 1.3577 Final absorption correction factors: Amin= 0.4784 Amax= 1.4788 PROFFIT INFO: Inet (after scale3 abspack): min=600.0842 max=4340609.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=132.8721 max=51918.5859 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4654 reflections read from tmp file 1090 reflections are rejected (1090 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 1 4 3 0 2 1 2 1 96 Initial Chi^2= 0.43035 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.85278 Current error model SIG(F2)^2 = 140.05*I_RAW + 0.00*I_BACK+(0.02302*)^2 Cycle 2, Chi^2= 1.00010 Current error model SIG(F2)^2 = 122.00*I_RAW + 0.00*I_BACK+(0.02073*)^2 Cycle 3, Chi^2= 0.99999 Current error model SIG(F2)^2 = 121.56*I_RAW + 0.00*I_BACK+(0.02082*)^2 Final Chi^2= 0.99999 Final error model SIG(F2)^2 = 121.56*I_RAW + 0.00*I_BACK+(0.02082*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4340610- 1033949 465 1679531.57 44.46 100.00 1033938- 558770 465 761387.22 36.79 100.00 558043- 239810 465 372813.57 35.42 100.00 239646- 144451 465 180106.24 30.82 100.00 144444- 115250 465 130487.21 24.51 100.00 115026- 81296 465 94447.24 18.68 100.00 81288- 62083 465 71909.78 15.91 100.00 62047- 4495 465 34700.25 11.12 99.78 4487- 2585 465 3361.76 4.38 93.12 2578- 600 469 1978.66 3.58 65.46 ------------------------------------------------------------------------------------ 4340610- 600 4654 332787.78 22.55 95.81 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 726134.70 35.95 100.00 1.41- 1.12 465 535199.27 28.00 99.57 1.12- 0.96 465 457804.44 27.23 96.99 0.96- 0.87 465 309059.56 23.13 94.41 0.87- 0.81 465 402970.74 26.67 99.35 0.81- 0.73 465 210300.35 18.35 96.56 0.73- 0.71 465 160390.84 17.06 91.18 0.71- 0.65 465 269241.13 21.18 95.91 0.65- 0.62 465 134008.60 13.90 89.68 0.62- 0.58 469 124559.43 14.12 94.46 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 332787.78 22.55 95.81 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 465 726134.70 35.95 100.00 4.82- 1.12 930 630666.98 31.97 99.78 4.82- 0.96 1395 573046.14 30.39 98.85 4.82- 0.87 1860 507049.49 28.58 97.74 4.82- 0.81 2325 486233.74 28.19 98.06 4.82- 0.73 2790 440244.84 26.55 97.81 4.82- 0.71 3255 400265.70 25.20 96.87 4.82- 0.65 3720 383887.63 24.70 96.75 4.82- 0.62 4185 356123.29 23.50 95.96 4.82- 0.58 4654 332787.78 22.55 95.81 ------------------------------------------------------------------------------------ 4.82- 0.58 4654 332787.78 22.55 95.81 Scale applied to data: s=0.230382 (maximum obs:4340609.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.052; Rsigma 0.028: data 4654 -> merged 110 With outlier rejection... Rint 0.051; Rsigma 0.028: data 4645 -> merged 110 Rejected total: 9, method kkm 7, method Blessing 2 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585468, 4.827892 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 29.90 100.00 299 1.61 - 1.21 10 10 43.30 100.00 433 1.17 - 1.01 10 10 55.40 100.00 554 0.99 - 0.89 10 10 53.60 100.00 536 0.88 - 0.81 10 10 51.10 100.00 511 0.81 - 0.74 10 10 44.70 100.00 447 0.73 - 0.71 10 10 49.30 100.00 493 0.70 - 0.66 10 10 40.70 100.00 407 0.65 - 0.64 10 10 38.20 100.00 382 0.63 - 0.60 10 10 36.60 100.00 366 --------------------------------------------------------------- 8.36 - 0.60 100 100 44.28 100.00 4428 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 16:52:45 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.357626 8.366248 8.362591 89.9665 89.9999 89.9657 4645 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.26 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2368 0 3115 3119 4645 N (int>3sigma) = 0 0 0 0 2368 0 2994 2987 4458 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.0 79.4 77.6 Mean int/sigma = 0.0 0.0 0.0 0.0 23.0 0.0 22.3 22.4 22.3 Lattice type: F chosen Volume: 584.73 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Unitcell: 5.911 5.911 5.911 90.03 119.94 119.98 Niggli form: a.a = 34.940 b.b = 34.946 c.c = 34.946 b.c = -0.021 a.c = -17.442 a.b = -17.462 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.050 CUBIC F-lattice R(int) = 0.049 [ 4488] Vol = 584.7 Cell: 8.363 8.366 8.358 90.03 90.00 90.03 Volume: 584.73 Matrix: 0.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.048 RHOMBOHEDRAL R-lattice R(int) = 0.054 [ 4204] Vol = 438.5 Cell: 5.913 5.911 14.489 90.03 90.03 120.01 Volume: 438.55 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.048 RHOMBOHEDRAL R-lattice R(int) = 0.048 [ 1342] Vol = 438.5 Trigonal Cell: 5.913 5.911 14.489 90.03 90.03 120.01 Volume: 438.55 Matrix: 0.0000 -0.5000 0.5000 0.5000 0.0000 -0.5000 1.0000 1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.020 TETRAGONAL I-lattice R(int) = 0.048 [ 4238] Vol = 292.4 Cell: 5.916 5.913 8.358 89.98 89.98 89.97 Volume: 292.36 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.042 TETRAGONAL I-lattice R(int) = 0.048 [ 4238] Vol = 292.4 Cell: 5.913 5.916 8.358 90.02 90.02 89.97 Volume: 292.36 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.019 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4184] Vol = 292.4 Cell: 5.913 5.916 8.358 89.98 89.98 89.97 Volume: 292.36 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.029 ORTHORHOMBIC I-lattice R(int) = 0.046 [ 4180] Vol = 292.4 Cell: 5.911 8.363 5.915 89.98 89.94 89.98 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.016 MONOCLINIC I-lattice R(int) = 0.046 [ 3830] Vol = 292.4 Cell: 5.916 5.913 8.358 90.02 90.02 89.97 Volume: 292.36 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.036 MONOCLINIC I-lattice R(int) = 0.045 [ 3828] Vol = 292.4 Cell: 5.911 5.915 8.363 90.02 90.02 89.94 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.020 MONOCLINIC I-lattice R(int) = 0.044 [ 3843] Vol = 292.4 Cell: 5.911 8.363 5.915 89.98 90.06 90.02 Volume: 292.36 Matrix:-0.5000 0.5000 0.0000 0.0000 0.0000 -1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [27] err= 0.029 MONOCLINIC I-lattice R(int) = 0.045 [ 3827] Vol = 292.4 Cell: 5.915 5.911 8.363 89.98 90.02 90.06 Volume: 292.36 Matrix: 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.027 MONOCLINIC C-lattice R(int) = 0.045 [ 3827] Vol = 292.4 Cell: 10.240 5.911 5.911 90.03 125.21 89.98 Volume: 292.36 Matrix: 0.5000 -1.0000 0.5000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.041 [ 3152] Vol = 146.2 Cell: 5.911 5.911 5.911 90.03 119.94 119.98 Volume: 146.18 Matrix: 0.5000 -0.5000 0.0000 -0.5000 0.0000 0.5000 -0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2368 0 3115 3126 4645 N (int>3sigma) = 0 0 0 0 2368 0 2994 3003 4458 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.0 78.5 77.6 Mean int/sigma = 0.0 0.0 0.0 0.0 23.0 0.0 22.3 22.4 22.3 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.162 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 50 50 355 1042 N I>3s 49 49 324 1042 1.0 1.0 0.7 36.6 8.6 8.6 5.2 25.7 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.049 4153 Fd-3m 1 1 227 C N N N N 37 2284 0.049 4192 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362591 8.366248 8.357626 90.0343 89.9999 90.0335 ZERR 3.00 0.000435 0.000517 0.000553 0.0052 0.0048 0.0047 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3717565- 477451 1034 1032 27 38.2 1150839.35 39.68 0.049 0.065 465582- 112324 1370 1368 27 50.7 198720.45 29.71 0.054 0.066 98711- 33126 1148 1148 27 42.5 72856.63 16.00 0.073 0.096 9737- 1763 1102 1097 29 37.8 3266.95 4.36 0.176 0.246 ------------------------------------------------------------------------------------------- 3717565- 1763 4654 4645 110 42.2 332990.11 22.55 0.051 0.067 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1190 1186 27 43.9 600518.03 32.09 0.047 0.066 0.023 1.01-0.78 1389 1388 27 51.4 313208.82 22.18 0.044 0.055 0.028 0.78-0.65 1199 1198 27 44.4 234258.51 19.28 0.061 0.075 0.034 0.65-0.59 876 873 29 30.1 136482.38 14.67 0.081 0.083 0.044 ------------------------------------------------------------------------------------------------------ inf-0.59 4654 4645 110 42.2 332990.11 22.55 0.051 0.067 0.028 inf-0.60 4433 4426 99 44.7 344969.98 23.04 0.051 0.067 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1186 27 27 100.0 43.9 600518.03 238.16 0.047 0.005 1.01-0.78 1388 27 27 100.0 51.4 313208.82 168.48 0.044 0.004 0.78-0.65 1198 27 27 100.0 44.4 234258.51 135.47 0.061 0.006 0.65-0.59 873 29 29 100.0 30.1 136482.38 92.68 0.081 0.011 -------------------------------------------------------------------------------------------- inf-0.59 4645 110 110 100.0 42.2 332990.11 163.51 0.051 0.006 inf-0.60 4426 99 99 100.0 44.7 344969.98 168.07 0.051 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC PROFFIT INFO: Meta algorithm block started Process information (Tue Mar 27 16:59:20 2018) ID: 2932; threads 39; handles 878; mem 518920.00 (1237720.00)kB; time: 1w 5d 2h 4m 51s MEMORY INFO: Memory PF:1.0, Ph:234.0, V:1208.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:506.8,peak PF: 697.1, WS: 297.0, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:93.2 (#24) MEMORY INFO: Tracker: RED 93.6 (#5) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) MEMORY INFO: Memory PF:3.0, Ph:234.0, V:1210.0; MEMORY INFO: Process info - Handles: 879, Memory: PF:508.5,peak PF: 697.1, WS: 298.8, peak WS: 556.7 MEMORY INFO: RED G:2.4,H:25.5 (#1096),V:95.0 (#25) MEMORY INFO: Tracker: RED 95.3 (#6) MEMORY INFO: Image pool: RED 6.0/100.0 (#6, page size: 4096) DC PROFFIT - Profile-fitting data reduction algorithm (39.29c (release 19-06-2017),compiled Jun 19 2017,17:34:21) DC PROFFIT - Started at Tue Mar 27 16:59:20 2018 Experiment file name: D:\Data\xs1714a\xs1714a Output file name: D:\Data\xs1714a\xs1714a Data reduction with automatic settings UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000005 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) 8.37024 ( 0.00055 ) 8.37691 ( 0.00052 ) 8.37554 ( 0.00044 ) 90.02113 ( 0.00468 ) 90.03240 ( 0.00484 ) 90.03043 ( 0.00519 ) V = 587.27 Selected cell (from UM rr/UM ttt/UM f): 1 8.3702 8.3769 8.3755 90.0211 90.0324 90.0304 cF Cross checking gral lattice... Lattice type F selected Background parameters (old style): 25 25 SHORT follow:0 DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_bg.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion1.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_ppcriterion2.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvsframe.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_predictaccuracyvstheta.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_profiles.dat) DELETE INFO: Deleting dat files... (D:\Data\xs1714a\plots_red\xs1714a_profilecorr*.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_latticeperrun.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_refinedsubmodels.dat) DELETE INFO: Deleting dat file... (D:\Data\xs1714a\plots_red\xs1714a_lattice.dat) DELETE INFO: Deleting ini file... 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(D:\Data\xs1714a\xs1714a.errmod) Per-frame model refinement: ON Instrument model dd at start: 52.84 mm Single frame average background scaling: OFF Dual wavelength al1-al2: ON 2-cycle 3D peak analysis: ON Background computed as FLOAT type: OFF Use 3D profile fitting: ON Adjust masks according to prediction uncertainty (for high angle data): OFF Follow profile size changes with incidence angle: ON Reject reflections with bad profiles: OFF Overflow threshold: 230000 Overflow marker: -9999999 Use JETSHADOW for masking shadowed areas: OFF Space group determination with Gral AutoChem attempted 0 Extinction conditions: PROFFITPEAK - Precise peak table update based on 3D profile analysis (2005-2015) PROFFITPEAK - Started at Tue Mar 27 16:59:20 2018 Experiment file name: D:\Data\xs1714a\xs1714a Maximum reflection width (in deg): 2.00 I/sigma threshold: 7.00 UB - matrix: -0.024968 -0.079420 -0.015593 ( 0.000005 0.000005 0.000005 ) 0.072431 -0.029136 0.032908 ( 0.000006 0.000006 0.000006 ) -0.036213 -0.003622 0.076458 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007203 -0.000004 -0.000000 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) -0.000000 -0.000004 0.007194 ( 0.000001 0.000001 0.000001 ) unit cell: 8.3702(5) 8.3769(5) 8.3755(4) 90.021(5) 90.032(5) 90.030(5) V = 587.27(6) unit cell: 8.36215(16) 8.36215(16) 8.36215(16) 90.0 90.0 90.0 V = 584.73(2) Lattice type F used *** 3D peak analysis started - run 1 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) UB fit with 594 obs out of 684 (total:685,skipped:1) (86.84%) UB - matrix: -0.024705 -0.079511 -0.015521 ( 0.000024 0.000020 0.000028 ) 0.072410 -0.028904 0.033042 ( 0.000026 0.000021 0.000030 ) -0.036209 -0.003584 0.076502 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007165 0.000001 0.000006 ( 0.000004 0.000003 0.000003 ) 0.000001 0.007170 0.000005 ( 0.000003 0.000003 0.000003 ) 0.000006 0.000005 0.007185 ( 0.000003 0.000003 0.000005 ) unit cell: 8.380(3) 8.376(2) 8.368(3) 90.04(2) 90.05(3) 90.01(2) V = 587.4(3) OTKP changes: 108 1 1 1 UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) UB - matrix: -0.024542 -0.079453 -0.015457 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028792 0.033000 ( 0.000025 0.000021 0.000030 ) -0.036195 -0.003488 0.076459 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007154 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007174 ( 0.000003 0.000003 0.000005 ) unit cell: 8.391(3) 8.386(2) 8.374(3) 90.09(2) 89.99(3) 89.95(2) V = 589.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.896) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024538 -0.079450 -0.015456 ( 0.000023 0.000019 0.000027 ) 0.072335 -0.028790 0.032998 ( 0.000025 0.000021 0.000030 ) -0.036196 -0.003487 0.076457 ( 0.000027 0.000023 0.000032 ) M - matrix: 0.007145 -0.000007 -0.000001 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007153 0.000011 ( 0.000003 0.000003 0.000003 ) -0.000001 0.000011 0.007173 ( 0.000003 0.000003 0.000005 ) UB fit with 593 obs out of 684 (total:685,skipped:1) (86.70%) unit cell: 8.392(3) 8.386(2) 8.375(3) 90.09(2) 89.99(3) 89.95(2) V = 589.4(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 595 obs out of 684 (total:685,skipped:1) (86.99%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 7 of 454 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 1.33 | 45 | 0.980 ( 0.174) | 1.321 ( 0.740) | 1.554 ( 2.296) | 1.33- 1.09 | 45 | 1.065 ( 0.113) | 1.089 ( 0.138) | 1.126 ( 0.494) | 1.09- 0.96 | 45 | 1.056 ( 0.114) | 1.074 ( 0.141) | 1.075 ( 0.398) | 0.94- 0.84 | 45 | 1.079 ( 0.109) | 1.068 ( 0.141) | 1.142 ( 0.397) | 0.84- 0.81 | 45 | 1.105 ( 0.100) | 1.019 ( 0.122) | 1.367 ( 0.510) | 0.78- 0.73 | 45 | 1.109 ( 0.081) | 0.988 ( 0.125) | 1.343 ( 0.487) | 0.73- 0.69 | 45 | 1.087 ( 0.080) | 0.931 ( 0.104) | 1.374 ( 0.529) | 0.69- 0.66 | 45 | 1.071 ( 0.075) | 0.888 ( 0.097) | 1.353 ( 0.457) | 0.66- 0.62 | 45 | 1.049 ( 0.074) | 0.850 ( 0.049) | 1.370 ( 0.600) | 0.62- 0.59 | 42 | 1.024 ( 0.086) | 0.807 ( 0.035) | 1.397 ( 0.570) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.73- 0.59 | 447 | 1.063 ( 0.111) | 1.005 ( 0.294) | 1.309 ( 0.879) | Optimal grid size for profile fitting: 9 x 9 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) UB - matrix: -0.024576 -0.079439 -0.015337 ( 0.000014 0.000011 0.000013 ) 0.072472 -0.028944 0.032943 ( 0.000014 0.000011 0.000013 ) -0.036034 -0.003354 0.076427 ( 0.000015 0.000012 0.000014 ) M - matrix: 0.007155 -0.000024 0.000010 ( 0.000002 0.000002 0.000002 ) -0.000024 0.007160 0.000009 ( 0.000002 0.000002 0.000002 ) 0.000010 0.000009 0.007162 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3858(13) 8.3828(12) 8.3816(14) 90.069(12) 90.083(13) 89.804(12) V = 589.19(16) OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) *** 3D peak analysis started - run 1 (2nd cycle) *** Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.913) HKL list info: 809 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007174 -0.000003 0.000010 ( 0.000002 0.000001 0.000002 ) -0.000003 0.007162 0.000005 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000005 0.007189 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.024649 -0.079494 -0.015425 ( 0.000012 0.000010 0.000012 ) 0.072535 -0.028811 0.033022 ( 0.000013 0.000011 0.000012 ) -0.036125 -0.003521 0.076556 ( 0.000013 0.000011 0.000012 ) M - matrix: 0.007168 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007168 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007168 ( 0.000000 0.000000 0.000001 ) UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) unit cell: 8.3744(12) 8.3815(11) 8.3655(12) 90.042(11) 90.079(12) 89.975(11) V = 587.17(14) unit cell: 8.3738(4) 8.3738(4) 8.3738(4) 90.0 90.0 90.0 V = 587.17(5) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 447 obs out of 447 (total:447,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb 8 of 449 peaks identified as outliers and rejected 441 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" 441 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1.tabbin file 441 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_1.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.32 | 44 | 0.983 ( 0.168) | 1.296 ( 0.708) | 1.556 ( 2.302) | 1.32- 1.09 | 44 | 1.064 ( 0.112) | 1.085 ( 0.140) | 1.170 ( 0.505) | 1.09- 0.96 | 44 | 1.062 ( 0.105) | 1.085 ( 0.144) | 1.116 ( 0.480) | 0.96- 0.85 | 44 | 1.073 ( 0.111) | 1.055 ( 0.136) | 1.146 ( 0.402) | 0.84- 0.81 | 44 | 1.114 ( 0.099) | 1.037 ( 0.130) | 1.328 ( 0.470) | 0.81- 0.73 | 44 | 1.088 ( 0.088) | 0.991 ( 0.129) | 1.303 ( 0.486) | 0.73- 0.70 | 44 | 1.095 ( 0.076) | 0.951 ( 0.114) | 1.397 ( 0.484) | 0.70- 0.67 | 44 | 1.078 ( 0.071) | 0.883 ( 0.071) | 1.433 ( 0.478) | 0.67- 0.63 | 44 | 1.070 ( 0.063) | 0.871 ( 0.063) | 1.445 ( 0.589) | 0.63- 0.59 | 45 | 1.013 ( 0.081) | 0.808 ( 0.036) | 1.283 ( 0.499) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 441 | 1.064 ( 0.108) | 1.006 ( 0.281) | 1.318 ( 0.874) | Optimal grid size for profile fitting: 9 x 9 *** 3D peak analysis started - run 2 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) UB - matrix: -0.024880 -0.079461 -0.015647 ( 0.000026 0.000031 0.000022 ) 0.072450 -0.029155 0.032841 ( 0.000029 0.000035 0.000024 ) -0.036188 -0.003658 0.076435 ( 0.000021 0.000025 0.000018 ) M - matrix: 0.007178 -0.000003 0.000003 ( 0.000005 0.000004 0.000003 ) -0.000003 0.007178 0.000006 ( 0.000004 0.000005 0.000003 ) 0.000003 0.000006 0.007166 ( 0.000003 0.000003 0.000003 ) unit cell: 8.372(3) 8.372(3) 8.379(2) 90.05(2) 90.02(2) 89.98(3) V = 587.3(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) UB - matrix: -0.024642 -0.079243 -0.015536 ( 0.000026 0.000030 0.000021 ) 0.072259 -0.028877 0.032792 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003637 0.076223 ( 0.000022 0.000026 0.000018 ) M - matrix: 0.007135 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007127 0.000007 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000007 0.007127 ( 0.000003 0.000003 0.000003 ) unit cell: 8.397(3) 8.402(3) 8.402(2) 90.06(2) 89.97(2) 89.98(3) V = 592.8(3) OTKP changes: 99 1 1 1 UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=53.113) HKL list info: 739 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024624 -0.079225 -0.015535 ( 0.000026 0.000031 0.000021 ) 0.072249 -0.028853 0.032785 ( 0.000029 0.000035 0.000024 ) -0.036150 -0.003634 0.076203 ( 0.000021 0.000025 0.000017 ) M - matrix: 0.007133 -0.000002 -0.000003 ( 0.000005 0.000004 0.000003 ) -0.000002 0.007122 0.000008 ( 0.000004 0.000005 0.000003 ) -0.000003 0.000008 0.007123 ( 0.000003 0.000003 0.000003 ) UB fit with 489 obs out of 535 (total:535,skipped:0) (91.40%) unit cell: 8.398(3) 8.405(3) 8.404(2) 90.06(2) 89.97(2) 89.98(3) V = 593.2(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 490 obs out of 535 (total:535,skipped:0) (91.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 4 of 413 peaks identified as outliers and rejected 409 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 409 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 409 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.33 | 41 | 0.969 ( 0.128) | 1.199 ( 0.565) | 1.144 ( 0.894) | 1.33- 1.09 | 41 | 1.022 ( 0.082) | 1.090 ( 0.105) | 1.048 ( 0.424) | 1.09- 0.96 | 41 | 1.017 ( 0.093) | 1.150 ( 0.396) | 1.037 ( 0.412) | 0.96- 0.86 | 41 | 1.002 ( 0.089) | 1.060 ( 0.137) | 1.092 ( 0.429) | 0.86- 0.81 | 41 | 1.019 ( 0.077) | 1.056 ( 0.133) | 1.058 ( 0.274) | 0.81- 0.73 | 41 | 0.977 ( 0.064) | 1.041 ( 0.152) | 1.094 ( 0.380) | 0.73- 0.70 | 41 | 0.973 ( 0.059) | 0.929 ( 0.112) | 1.062 ( 0.430) | 0.69- 0.66 | 41 | 0.960 ( 0.040) | 0.905 ( 0.085) | 1.221 ( 0.446) | 0.66- 0.63 | 41 | 0.922 ( 0.030) | 0.858 ( 0.065) | 1.207 ( 0.478) | 0.63- 0.59 | 40 | 0.898 ( 0.037) | 0.834 ( 0.060) | 1.279 ( 0.458) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 409 | 0.976 ( 0.085) | 1.013 ( 0.267) | 1.124 ( 0.494) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) UB - matrix: -0.024706 -0.079343 -0.015462 ( 0.000013 0.000014 0.000010 ) 0.072163 -0.028887 0.032874 ( 0.000015 0.000017 0.000013 ) -0.036322 -0.003695 0.076125 ( 0.000012 0.000013 0.000009 ) M - matrix: 0.007137 0.000010 -0.000011 ( 0.000002 0.000002 0.000001 ) 0.000010 0.007143 -0.000004 ( 0.000002 0.000002 0.000001 ) -0.000011 -0.000004 0.007115 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3959(14) 8.3923(14) 8.4091(11) 89.967(12) 89.914(12) 90.079(14) V = 592.51(16) OTKP changes: 409 1 1 1 No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) *** 3D peak analysis started - run 2 (2nd cycle) *** Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.926) HKL list info: 731 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007176 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007184 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000003 0.000000 0.007167 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024798 -0.079514 -0.015577 ( 0.000012 0.000013 0.000010 ) 0.072429 -0.029116 0.032887 ( 0.000014 0.000016 0.000012 ) -0.036257 -0.003676 0.076438 ( 0.000010 0.000011 0.000008 ) M - matrix: 0.007171 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007171 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007171 ( 0.000000 0.000000 0.000001 ) UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) unit cell: 8.3734(13) 8.3687(13) 8.3785(9) 90.001(11) 89.975(11) 89.970(13) V = 587.12(15) unit cell: 8.3735(3) 8.3735(3) 8.3735(3) 90.0 90.0 90.0 V = 587.12(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 409 obs out of 409 (total:409,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb 3 of 409 peaks identified as outliers and rejected 406 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" 406 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2.tabbin file 406 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_2.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 1.32 | 41 | 0.991 ( 0.137) | 1.259 ( 0.667) | 1.211 ( 0.942) | 1.32- 1.09 | 41 | 1.028 ( 0.083) | 1.100 ( 0.098) | 1.066 ( 0.413) | 1.09- 0.94 | 41 | 1.025 ( 0.085) | 1.151 ( 0.366) | 1.098 ( 0.464) | 0.94- 0.84 | 41 | 1.000 ( 0.089) | 1.049 ( 0.144) | 1.024 ( 0.343) | 0.84- 0.81 | 41 | 1.005 ( 0.089) | 1.042 ( 0.146) | 1.024 ( 0.267) | 0.78- 0.73 | 41 | 0.993 ( 0.055) | 1.047 ( 0.147) | 1.125 ( 0.417) | 0.73- 0.69 | 41 | 0.968 ( 0.057) | 0.930 ( 0.118) | 1.175 ( 0.562) | 0.69- 0.65 | 41 | 0.962 ( 0.041) | 0.907 ( 0.088) | 1.241 ( 0.474) | 0.65- 0.62 | 41 | 0.921 ( 0.026) | 0.853 ( 0.042) | 1.240 ( 0.473) | 0.62- 0.59 | 37 | 0.893 ( 0.035) | 0.829 ( 0.060) | 1.254 ( 0.471) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.77- 0.59 | 406 | 0.979 ( 0.087) | 1.018 ( 0.292) | 1.145 ( 0.519) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 3 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024955 -0.079489 -0.015519 ( 0.000031 0.000032 0.000024 ) 0.072506 -0.029251 0.032981 ( 0.000022 0.000023 0.000017 ) -0.036210 -0.003585 0.076440 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000011 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007187 -0.000005 ( 0.000003 0.000005 0.000003 ) 0.000011 -0.000005 0.007172 ( 0.000003 0.000003 0.000003 ) unit cell: 8.364(2) 8.367(3) 8.376(2) 89.96(2) 90.09(2) 89.94(2) V = 586.2(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) UB - matrix: -0.024990 -0.079508 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072489 -0.029278 0.032955 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003558 0.076487 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007191 -0.000007 0.000007 ( 0.000004 0.000003 0.000003 ) -0.000007 0.007191 -0.000004 ( 0.000003 0.000005 0.000003 ) 0.000007 -0.000004 0.007177 ( 0.000003 0.000003 0.000003 ) unit cell: 8.365(2) 8.364(3) 8.373(2) 89.97(2) 90.05(2) 89.95(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.024996 -0.079510 -0.015512 ( 0.000031 0.000032 0.000024 ) 0.072484 -0.029282 0.032950 ( 0.000022 0.000023 0.000017 ) -0.036214 -0.003553 0.076495 ( 0.000026 0.000027 0.000020 ) M - matrix: 0.007190 -0.000006 0.000006 ( 0.000004 0.000003 0.000003 ) -0.000006 0.007192 -0.000003 ( 0.000003 0.000005 0.000003 ) 0.000006 -0.000003 0.007178 ( 0.000003 0.000003 0.000003 ) UB fit with 571 obs out of 641 (total:641,skipped:0) (89.08%) unit cell: 8.365(2) 8.364(3) 8.372(2) 89.97(2) 90.05(2) 89.95(2) V = 585.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 566 obs out of 641 (total:641,skipped:0) (88.30%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 8 of 480 peaks identified as outliers and rejected 472 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 472 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 472 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 1.41 | 47 | 1.001 ( 0.127) | 1.120 ( 0.425) | 1.121 ( 0.599) | 1.41- 1.16 | 47 | 1.041 ( 0.138) | 1.186 ( 0.591) | 0.936 ( 0.358) | 1.16- 0.98 | 47 | 0.998 ( 0.092) | 1.018 ( 0.139) | 1.012 ( 0.462) | 0.98- 0.91 | 47 | 1.021 ( 0.080) | 1.016 ( 0.117) | 1.096 ( 0.437) | 0.89- 0.82 | 47 | 1.011 ( 0.070) | 0.991 ( 0.110) | 1.121 ( 0.389) | 0.82- 0.75 | 47 | 0.993 ( 0.082) | 0.958 ( 0.117) | 1.089 ( 0.435) | 0.75- 0.71 | 47 | 0.980 ( 0.044) | 0.915 ( 0.068) | 1.233 ( 0.517) | 0.71- 0.66 | 47 | 0.952 ( 0.050) | 0.859 ( 0.053) | 1.232 ( 0.481) | 0.66- 0.62 | 47 | 0.931 ( 0.045) | 0.843 ( 0.040) | 1.149 ( 0.408) | 0.62- 0.59 | 49 | 0.904 ( 0.042) | 0.810 ( 0.034) | 1.356 ( 0.585) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.76- 0.59 | 472 | 0.983 ( 0.093) | 0.971 ( 0.270) | 1.135 ( 0.487) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 471 obs out of 472 (total:472,skipped:0) (99.79%) UB - matrix: -0.025006 -0.079675 -0.015487 ( 0.000018 0.000016 0.000013 ) 0.072517 -0.029210 0.033108 ( 0.000012 0.000011 0.000009 ) -0.036211 -0.003638 0.076593 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 0.000006 0.000015 ( 0.000002 0.000002 0.000001 ) 0.000006 0.007214 -0.000012 ( 0.000002 0.000003 0.000001 ) 0.000015 -0.000012 0.007203 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3619(12) 8.3508(15) 8.3577(11) 89.906(13) 90.117(11) 90.047(13) V = 583.61(15) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) *** 3D peak analysis started - run 3 (2nd cycle) *** Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.838) HKL list info: 795 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007192 -0.000004 0.000001 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007190 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000001 -0.000008 0.007182 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025012 -0.079493 -0.015505 ( 0.000016 0.000014 0.000012 ) 0.072466 -0.029291 0.032954 ( 0.000010 0.000009 0.000007 ) -0.036268 -0.003596 0.076523 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007182 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007182 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007182 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) unit cell: 8.3637(11) 8.3650(14) 8.3696(11) 89.937(12) 90.005(10) 89.969(12) V = 585.56(14) unit cell: 8.3661(3) 8.3661(3) 8.3661(3) 90.0 90.0 90.0 V = 585.56(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 472 (total:472,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb 7 of 489 peaks identified as outliers and rejected 482 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" 482 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3.tabbin file 482 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_3.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 48 | 1.017 ( 0.238) | 1.199 ( 0.651) | 1.104 ( 0.625) | 1.48- 1.17 | 48 | 1.037 ( 0.129) | 1.139 ( 0.445) | 0.967 ( 0.489) | 1.17- 1.01 | 48 | 1.002 ( 0.088) | 1.041 ( 0.221) | 1.001 ( 0.450) | 1.01- 0.92 | 48 | 1.015 ( 0.075) | 1.018 ( 0.104) | 1.089 ( 0.445) | 0.92- 0.82 | 48 | 1.003 ( 0.084) | 0.983 ( 0.113) | 1.107 ( 0.381) | 0.82- 0.75 | 48 | 0.996 ( 0.081) | 0.965 ( 0.114) | 1.091 ( 0.434) | 0.75- 0.71 | 48 | 0.989 ( 0.045) | 0.920 ( 0.067) | 1.217 ( 0.500) | 0.71- 0.67 | 48 | 0.951 ( 0.048) | 0.862 ( 0.057) | 1.211 ( 0.484) | 0.67- 0.62 | 48 | 0.936 ( 0.047) | 0.847 ( 0.039) | 1.203 ( 0.420) | 0.62- 0.59 | 50 | 0.903 ( 0.042) | 0.812 ( 0.037) | 1.355 ( 0.583) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 482 | 0.984 ( 0.111) | 0.978 ( 0.293) | 1.136 ( 0.499) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 4 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) UB fit with 579 obs out of 669 (total:669,skipped:0) (86.55%) UB - matrix: -0.025004 -0.079560 -0.015634 ( 0.000020 0.000029 0.000031 ) 0.072332 -0.029282 0.032890 ( 0.000019 0.000027 0.000029 ) -0.036200 -0.003682 0.076472 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007168 0.000005 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000005 0.007201 -0.000001 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000001 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.378(2) 8.359(3) 8.374(3) 89.99(3) 90.01(2) 90.04(2) V = 586.5(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 577 obs out of 669 (total:669,skipped:0) (86.25%) UB - matrix: -0.025006 -0.079582 -0.015615 ( 0.000020 0.000029 0.000030 ) 0.072323 -0.029314 0.032900 ( 0.000018 0.000027 0.000029 ) -0.036195 -0.003670 0.076471 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007166 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007206 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) unit cell: 8.379(2) 8.356(3) 8.374(3) 89.98(3) 90.02(2) 90.02(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 796 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025009 -0.079586 -0.015615 ( 0.000019 0.000028 0.000030 ) 0.072319 -0.029315 0.032895 ( 0.000018 0.000027 0.000028 ) -0.036193 -0.003671 0.076474 ( 0.000020 0.000029 0.000031 ) M - matrix: 0.007165 0.000003 0.000002 ( 0.000003 0.000003 0.000003 ) 0.000003 0.007207 -0.000002 ( 0.000003 0.000005 0.000004 ) 0.000002 -0.000002 0.007174 ( 0.000003 0.000004 0.000005 ) UB fit with 575 obs out of 669 (total:669,skipped:0) (85.95%) unit cell: 8.379(2) 8.355(3) 8.374(3) 89.98(3) 90.01(2) 90.03(2) V = 586.3(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 580 obs out of 669 (total:669,skipped:0) (86.70%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 11 of 481 peaks identified as outliers and rejected 470 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 470 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 470 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.40 | 47 | 1.041 ( 0.148) | 1.139 ( 0.454) | 1.142 ( 0.826) | 1.40- 1.12 | 47 | 1.046 ( 0.106) | 1.246 ( 0.549) | 1.080 ( 0.618) | 1.12- 0.96 | 47 | 1.023 ( 0.104) | 1.048 ( 0.128) | 0.910 ( 0.315) | 0.96- 0.89 | 47 | 1.027 ( 0.095) | 1.019 ( 0.138) | 1.125 ( 0.416) | 0.88- 0.82 | 47 | 1.048 ( 0.080) | 1.019 ( 0.119) | 1.194 ( 0.513) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.984 ( 0.120) | 1.154 ( 0.469) | 0.75- 0.71 | 47 | 1.022 ( 0.047) | 0.930 ( 0.111) | 1.336 ( 0.533) | 0.71- 0.67 | 47 | 1.000 ( 0.041) | 0.888 ( 0.071) | 1.195 ( 0.468) | 0.67- 0.62 | 47 | 0.973 ( 0.047) | 0.839 ( 0.041) | 1.275 ( 0.503) | 0.62- 0.59 | 47 | 0.949 ( 0.045) | 0.812 ( 0.043) | 1.361 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 470 | 1.017 ( 0.092) | 0.992 ( 0.275) | 1.177 ( 0.548) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 468 obs out of 470 (total:470,skipped:0) (99.57%) UB - matrix: -0.024932 -0.079612 -0.015778 ( 0.000008 0.000013 0.000013 ) 0.072566 -0.029286 0.032953 ( 0.000010 0.000017 0.000017 ) -0.036186 -0.003596 0.076549 ( 0.000008 0.000013 0.000013 ) M - matrix: 0.007197 -0.000010 0.000015 ( 0.000002 0.000002 0.000002 ) -0.000010 0.007209 0.000016 ( 0.000002 0.000002 0.000002 ) 0.000015 0.000016 0.007195 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3611(12) 8.3541(13) 8.3624(12) 90.126(12) 90.117(12) 89.919(13) V = 584.11(15) OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 OTKP changes: 469 1 1 1 No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) *** 3D peak analysis started - run 4 (2nd cycle) *** Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.838) HKL list info: 793 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007175 0.000003 0.000004 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007193 -0.000000 ( 0.000001 0.000002 0.000001 ) 0.000004 -0.000000 0.007188 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025087 -0.079479 -0.015714 ( 0.000008 0.000013 0.000012 ) 0.072343 -0.029366 0.032928 ( 0.000008 0.000013 0.000013 ) -0.036229 -0.003688 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) unit cell: 8.3735(10) 8.3633(12) 8.3660(11) 89.998(11) 90.029(10) 90.024(11) V = 585.87(13) unit cell: 8.3676(3) 8.3676(3) 8.3676(3) 90.0 90.0 90.0 V = 585.87(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 469 obs out of 470 (total:470,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb 8 of 479 peaks identified as outliers and rejected 471 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" 471 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4.tabbin file 471 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_4.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 47 | 1.022 ( 0.154) | 1.112 ( 0.427) | 1.061 ( 0.753) | 1.41- 1.12 | 47 | 1.058 ( 0.097) | 1.230 ( 0.561) | 1.118 ( 0.641) | 1.12- 0.97 | 47 | 1.016 ( 0.108) | 1.031 ( 0.129) | 0.976 ( 0.366) | 0.96- 0.89 | 47 | 1.030 ( 0.090) | 1.030 ( 0.137) | 1.095 ( 0.390) | 0.88- 0.82 | 47 | 1.049 ( 0.080) | 1.023 ( 0.118) | 1.207 ( 0.510) | 0.82- 0.75 | 47 | 1.039 ( 0.080) | 0.983 ( 0.123) | 1.092 ( 0.429) | 0.75- 0.71 | 47 | 1.024 ( 0.044) | 0.940 ( 0.115) | 1.318 ( 0.539) | 0.71- 0.67 | 47 | 0.999 ( 0.043) | 0.885 ( 0.072) | 1.212 ( 0.465) | 0.67- 0.62 | 47 | 0.975 ( 0.047) | 0.842 ( 0.042) | 1.287 ( 0.500) | 0.62- 0.59 | 48 | 0.948 ( 0.045) | 0.812 ( 0.043) | 1.348 ( 0.526) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 471 | 1.016 ( 0.092) | 0.988 ( 0.270) | 1.172 ( 0.536) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 5 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) UB fit with 496 obs out of 550 (total:550,skipped:0) (90.18%) UB - matrix: -0.025203 -0.079378 -0.015755 ( 0.000024 0.000034 0.000034 ) 0.072368 -0.029302 0.032817 ( 0.000017 0.000024 0.000024 ) -0.036239 -0.003642 0.076546 ( 0.000019 0.000026 0.000026 ) M - matrix: 0.007186 0.000012 -0.000002 ( 0.000003 0.000003 0.000003 ) 0.000012 0.007173 0.000010 ( 0.000003 0.000006 0.000004 ) -0.000002 0.000010 0.007184 ( 0.000003 0.000004 0.000004 ) unit cell: 8.368(2) 8.375(3) 8.368(2) 90.08(3) 89.98(2) 90.10(2) V = 586.4(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) UB - matrix: -0.025278 -0.079338 -0.015744 ( 0.000025 0.000035 0.000036 ) 0.072351 -0.029354 0.032796 ( 0.000016 0.000023 0.000023 ) -0.036147 -0.003626 0.076574 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007180 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000009 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000009 0.007187 ( 0.000003 0.000004 0.000005 ) unit cell: 8.371(2) 8.377(3) 8.367(2) 90.07(3) 90.02(2) 90.10(2) V = 586.7(3) OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 OTKP changes: 98 1 1 1 UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 745 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025280 -0.079338 -0.015740 ( 0.000025 0.000035 0.000036 ) 0.072355 -0.029355 0.032795 ( 0.000016 0.000023 0.000023 ) -0.036142 -0.003628 0.076575 ( 0.000019 0.000027 0.000028 ) M - matrix: 0.007181 0.000013 0.000003 ( 0.000003 0.000003 0.000003 ) 0.000013 0.007169 0.000008 ( 0.000003 0.000006 0.000004 ) 0.000003 0.000008 0.007187 ( 0.000003 0.000004 0.000005 ) UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) unit cell: 8.370(2) 8.377(3) 8.367(2) 90.07(3) 90.03(2) 90.10(2) V = 586.7(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 506 obs out of 550 (total:550,skipped:0) (92.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 2 of 449 peaks identified as outliers and rejected 447 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 447 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 447 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 1.48 | 45 | 0.992 ( 0.190) | 1.208 ( 0.637) | 1.144 ( 0.739) | 1.47- 1.17 | 45 | 1.017 ( 0.089) | 1.091 ( 0.327) | 0.975 ( 0.390) | 1.17- 0.98 | 45 | 1.009 ( 0.082) | 1.040 ( 0.167) | 0.992 ( 0.453) | 0.98- 0.91 | 45 | 1.006 ( 0.080) | 1.005 ( 0.115) | 1.040 ( 0.386) | 0.91- 0.82 | 45 | 1.013 ( 0.066) | 0.975 ( 0.103) | 1.231 ( 0.531) | 0.82- 0.75 | 45 | 0.995 ( 0.078) | 0.971 ( 0.123) | 1.145 ( 0.429) | 0.75- 0.71 | 45 | 0.974 ( 0.048) | 0.925 ( 0.065) | 1.258 ( 0.463) | 0.71- 0.67 | 45 | 0.950 ( 0.043) | 0.870 ( 0.065) | 1.297 ( 0.563) | 0.67- 0.62 | 45 | 0.913 ( 0.034) | 0.841 ( 0.046) | 1.390 ( 0.528) | 0.62- 0.59 | 42 | 0.885 ( 0.033) | 0.813 ( 0.039) | 1.417 ( 0.626) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.78- 0.59 | 447 | 0.976 ( 0.096) | 0.975 ( 0.269) | 1.187 ( 0.541) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 445 obs out of 447 (total:447,skipped:0) (99.55%) UB - matrix: -0.025224 -0.079521 -0.015770 ( 0.000011 0.000016 0.000017 ) 0.072408 -0.029418 0.032773 ( 0.000007 0.000011 0.000011 ) -0.036329 -0.003648 0.076603 ( 0.000009 0.000013 0.000014 ) M - matrix: 0.007199 0.000008 -0.000012 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007202 0.000010 ( 0.000001 0.000003 0.000002 ) -0.000012 0.000010 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3598(10) 8.3578(15) 8.3645(12) 90.083(13) 89.904(11) 90.066(12) V = 584.43(15) OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 OTKP changes: 446 1 1 1 No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) *** 3D peak analysis started - run 5 (2nd cycle) *** Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.838) HKL list info: 746 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007186 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007184 0.000007 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000007 0.007192 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025268 -0.079407 -0.015727 ( 0.000011 0.000016 0.000017 ) 0.072379 -0.029421 0.032790 ( 0.000008 0.000012 0.000012 ) -0.036181 -0.003623 0.076611 ( 0.000007 0.000011 0.000012 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) unit cell: 8.3671(10) 8.3684(14) 8.3640(11) 90.052(12) 89.990(10) 90.064(12) V = 585.64(14) unit cell: 8.3665(3) 8.3665(3) 8.3665(3) 90.0 90.0 90.0 V = 585.64(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 446 obs out of 447 (total:447,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb 3 of 454 peaks identified as outliers and rejected 451 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" 451 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5.tabbin file 451 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_5.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.48 | 45 | 0.992 ( 0.212) | 1.244 ( 0.702) | 1.167 ( 0.805) | 1.48- 1.17 | 45 | 1.025 ( 0.081) | 1.061 ( 0.115) | 1.020 ( 0.414) | 1.17- 0.98 | 45 | 1.005 ( 0.083) | 1.047 ( 0.122) | 0.950 ( 0.392) | 0.98- 0.92 | 45 | 1.003 ( 0.083) | 1.005 ( 0.117) | 1.017 ( 0.405) | 0.92- 0.82 | 45 | 1.011 ( 0.070) | 0.967 ( 0.103) | 1.287 ( 0.513) | 0.82- 0.76 | 45 | 0.998 ( 0.079) | 0.979 ( 0.124) | 1.124 ( 0.436) | 0.75- 0.71 | 45 | 0.975 ( 0.049) | 0.933 ( 0.076) | 1.239 ( 0.465) | 0.71- 0.67 | 45 | 0.953 ( 0.044) | 0.878 ( 0.065) | 1.224 ( 0.508) | 0.67- 0.62 | 45 | 0.916 ( 0.033) | 0.844 ( 0.044) | 1.415 ( 0.527) | 0.62- 0.59 | 46 | 0.887 ( 0.033) | 0.814 ( 0.038) | 1.429 ( 0.617) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 451 | 0.976 ( 0.100) | 0.977 ( 0.267) | 1.188 ( 0.545) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 6 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) UB fit with 577 obs out of 650 (total:650,skipped:0) (88.77%) UB - matrix: -0.025244 -0.079378 -0.015665 ( 0.000023 0.000017 0.000019 ) 0.072473 -0.029378 0.032812 ( 0.000034 0.000025 0.000029 ) -0.036106 -0.003515 0.076522 ( 0.000028 0.000020 0.000023 ) M - matrix: 0.007193 0.000002 0.000011 ( 0.000005 0.000003 0.000003 ) 0.000002 0.007176 0.000011 ( 0.000003 0.000003 0.000002 ) 0.000011 0.000011 0.007178 ( 0.000003 0.000002 0.000004 ) unit cell: 8.363(3) 8.3730(19) 8.372(2) 90.08(2) 90.08(3) 90.01(2) V = 586.3(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 UB fit with 589 obs out of 650 (total:650,skipped:0) (90.62%) UB - matrix: -0.025280 -0.079382 -0.015687 ( 0.000023 0.000017 0.000019 ) 0.072487 -0.029419 0.032784 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003485 0.076560 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 0.000000 0.000010 ( 0.000005 0.000003 0.000003 ) 0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000010 0.000014 0.007182 ( 0.000003 0.000003 0.000004 ) unit cell: 8.361(3) 8.3713(19) 8.369(3) 90.11(2) 90.08(3) 90.00(2) V = 585.8(3) OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 OTKP changes: 108 1 1 1 Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 797 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025282 -0.079382 -0.015688 ( 0.000023 0.000017 0.000019 ) 0.072486 -0.029425 0.032778 ( 0.000033 0.000024 0.000028 ) -0.036093 -0.003480 0.076567 ( 0.000029 0.000021 0.000025 ) M - matrix: 0.007196 -0.000000 0.000009 ( 0.000005 0.000003 0.000003 ) -0.000000 0.007179 0.000014 ( 0.000003 0.000003 0.000003 ) 0.000009 0.000014 0.007183 ( 0.000003 0.000003 0.000004 ) UB fit with 588 obs out of 650 (total:650,skipped:0) (90.46%) unit cell: 8.361(3) 8.3712(19) 8.369(3) 90.11(2) 90.07(3) 90.00(2) V = 585.8(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 582 obs out of 650 (total:650,skipped:0) (89.54%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 5 of 481 peaks identified as outliers and rejected 476 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 476 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 476 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 1.41 | 48 | 1.022 ( 0.151) | 1.235 ( 0.590) | 1.203 ( 0.914) | 1.41- 1.17 | 48 | 1.016 ( 0.110) | 1.145 ( 0.403) | 1.056 ( 0.556) | 1.17- 0.98 | 48 | 1.000 ( 0.089) | 1.126 ( 0.310) | 0.949 ( 0.377) | 0.98- 0.91 | 48 | 1.017 ( 0.076) | 1.048 ( 0.107) | 1.052 ( 0.429) | 0.91- 0.82 | 48 | 0.999 ( 0.081) | 1.001 ( 0.108) | 1.092 ( 0.376) | 0.82- 0.75 | 48 | 0.987 ( 0.067) | 0.974 ( 0.109) | 1.140 ( 0.437) | 0.75- 0.71 | 48 | 0.966 ( 0.051) | 0.904 ( 0.083) | 1.216 ( 0.467) | 0.71- 0.67 | 48 | 0.948 ( 0.045) | 0.883 ( 0.069) | 1.229 ( 0.443) | 0.67- 0.62 | 48 | 0.922 ( 0.040) | 0.847 ( 0.069) | 1.293 ( 0.462) | 0.62- 0.59 | 44 | 0.904 ( 0.044) | 0.820 ( 0.044) | 1.338 ( 0.515) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.81- 0.59 | 476 | 0.979 ( 0.091) | 1.000 ( 0.290) | 1.155 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) UB - matrix: -0.025277 -0.079584 -0.015535 ( 0.000015 0.000012 0.000015 ) 0.072557 -0.029408 0.032788 ( 0.000014 0.000011 0.000014 ) -0.036185 -0.003545 0.076566 ( 0.000013 0.000010 0.000013 ) M - matrix: 0.007213 0.000006 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000006 0.007211 0.000001 ( 0.000002 0.000002 0.000002 ) 0.000001 0.000001 0.007179 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3518(13) 8.3528(12) 8.3715(13) 90.005(12) 90.009(13) 90.049(13) V = 584.01(15) OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 OTKP changes: 475 1 1 1 No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) *** 3D peak analysis started - run 6 (2nd cycle) *** Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.838) HKL list info: 798 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007185 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007182 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007190 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025323 -0.079373 -0.015694 ( 0.000010 0.000008 0.000010 ) 0.072398 -0.029480 0.032783 ( 0.000014 0.000011 0.000014 ) -0.036089 -0.003534 0.076611 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007180 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007180 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007180 ( 0.000000 0.000000 0.000001 ) UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) unit cell: 8.3678(13) 8.3699(8) 8.3648(12) 90.068(10) 90.048(12) 90.026(10) V = 585.85(14) unit cell: 8.3675(3) 8.3675(3) 8.3675(3) 90.0 90.0 90.0 V = 585.85(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 475 obs out of 476 (total:476,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb 6 of 479 peaks identified as outliers and rejected 473 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" 473 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6.tabbin file 473 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_6.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 1.41 | 47 | 1.035 ( 0.188) | 1.258 ( 0.666) | 1.217 ( 0.904) | 1.41- 1.17 | 47 | 1.029 ( 0.094) | 1.167 ( 0.383) | 1.054 ( 0.551) | 1.17- 1.01 | 47 | 0.988 ( 0.098) | 1.051 ( 0.134) | 0.942 ( 0.384) | 1.01- 0.92 | 47 | 1.034 ( 0.069) | 1.084 ( 0.126) | 1.068 ( 0.494) | 0.92- 0.82 | 47 | 0.989 ( 0.082) | 0.993 ( 0.107) | 1.083 ( 0.390) | 0.82- 0.75 | 47 | 0.987 ( 0.071) | 0.977 ( 0.113) | 1.118 ( 0.418) | 0.75- 0.71 | 47 | 0.969 ( 0.052) | 0.908 ( 0.086) | 1.243 ( 0.482) | 0.71- 0.67 | 47 | 0.953 ( 0.040) | 0.890 ( 0.052) | 1.195 ( 0.402) | 0.67- 0.62 | 47 | 0.921 ( 0.043) | 0.843 ( 0.057) | 1.305 ( 0.462) | 0.62- 0.59 | 50 | 0.906 ( 0.043) | 0.826 ( 0.060) | 1.290 ( 0.512) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.84- 0.59 | 473 | 0.981 ( 0.098) | 0.999 ( 0.290) | 1.153 ( 0.532) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 7 *** Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 1.41 | 39 | 1.034 ( 0.140) | 1.212 ( 0.488) | 1.144 ( 0.710) | 1.41- 1.17 | 39 | 1.017 ( 0.109) | 1.175 ( 0.516) | 1.084 ( 0.530) | 1.17- 0.99 | 39 | 1.025 ( 0.094) | 1.047 ( 0.109) | 0.944 ( 0.361) | 0.99- 0.89 | 39 | 1.018 ( 0.096) | 1.012 ( 0.121) | 1.026 ( 0.379) | 0.89- 0.82 | 39 | 1.019 ( 0.086) | 1.008 ( 0.096) | 1.145 ( 0.483) | 0.82- 0.75 | 39 | 1.007 ( 0.087) | 0.964 ( 0.126) | 1.064 ( 0.402) | 0.75- 0.71 | 39 | 0.968 ( 0.066) | 0.899 ( 0.082) | 1.221 ( 0.547) | 0.71- 0.67 | 39 | 0.965 ( 0.044) | 0.877 ( 0.053) | 1.246 ( 0.535) | 0.67- 0.63 | 39 | 0.948 ( 0.039) | 0.830 ( 0.043) | 1.280 ( 0.452) | 0.63- 0.59 | 43 | 0.909 ( 0.040) | 0.782 ( 0.038) | 1.129 ( 0.419) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.83- 0.59 | 394 | 0.990 ( 0.094) | 0.978 ( 0.273) | 1.128 ( 0.501) | Optimal grid size for profile fitting: 7 x 7 *** 3D peak analysis started - run 8 *** BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Creating background file D:\Data\xs1714a\tmp\xs1714a_back_8_76.img BACKGROUND INFO: Creating background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_76.img BACKGROUND INFO: Creating background info file D:\Data\xs1714a\tmp\xs1714a_back_8_76.rpb PROFFITPEAK info: 1139 peaks in the peak location table UB fit with 513 obs out of 563 (total:563,skipped:0) (91.12%) UB - matrix: -0.025369 -0.079292 -0.015606 ( 0.000033 0.000026 0.000032 ) 0.072393 -0.029484 0.032787 ( 0.000024 0.000019 0.000024 ) -0.036266 -0.003704 0.076549 ( 0.000025 0.000020 0.000024 ) M - matrix: 0.007200 0.000011 -0.000007 ( 0.000004 0.000003 0.000003 ) 0.000011 0.007170 -0.000013 ( 0.000003 0.000004 0.000003 ) -0.000007 -0.000013 0.007178 ( 0.000003 0.000003 0.000004 ) unit cell: 8.359(2) 8.377(3) 8.372(2) 89.90(2) 89.95(2) 90.09(2) V = 586.2(3) UB fit with 513 obs out of 563 (total:563,skipped:0) (91.12%) UB - matrix: -0.025369 -0.079292 -0.015606 ( 0.000033 0.000026 0.000032 ) 0.072393 -0.029484 0.032787 ( 0.000024 0.000019 0.000024 ) -0.036266 -0.003704 0.076549 ( 0.000025 0.000020 0.000024 ) M - matrix: 0.007200 0.000011 -0.000007 ( 0.000004 0.000003 0.000003 ) 0.000011 0.007170 -0.000013 ( 0.000003 0.000004 0.000003 ) -0.000007 -0.000013 0.007178 ( 0.000003 0.000003 0.000004 ) unit cell: 8.359(2) 8.377(3) 8.372(2) 89.90(2) 89.95(2) 90.09(2) V = 586.2(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 UB - matrix: -0.025385 -0.079246 -0.015640 ( 0.000033 0.000026 0.000031 ) 0.072366 -0.029543 0.032811 ( 0.000025 0.000019 0.000023 ) -0.036334 -0.003651 0.076509 ( 0.000025 0.000020 0.000024 ) M - matrix: 0.007201 0.000006 -0.000008 ( 0.000004 0.000003 0.000003 ) 0.000006 0.007166 -0.000009 ( 0.000003 0.000004 0.000003 ) -0.000008 -0.000009 0.007175 ( 0.000003 0.000003 0.000004 ) UB fit with 518 obs out of 563 (total:563,skipped:0) (92.01%) unit cell: 8.358(2) 8.379(3) 8.374(2) 89.93(2) 89.93(2) 90.05(2) V = 586.5(3) UB fit with 518 obs out of 563 (total:563,skipped:0) (92.01%) UB - matrix: -0.025385 -0.079246 -0.015640 ( 0.000033 0.000026 0.000031 ) 0.072366 -0.029543 0.032811 ( 0.000025 0.000019 0.000023 ) -0.036334 -0.003651 0.076509 ( 0.000025 0.000020 0.000024 ) M - matrix: 0.007201 0.000006 -0.000008 ( 0.000004 0.000003 0.000003 ) 0.000006 0.007166 -0.000009 ( 0.000003 0.000004 0.000003 ) -0.000008 -0.000009 0.007175 ( 0.000003 0.000003 0.000004 ) unit cell: 8.358(2) 8.379(3) 8.374(2) 89.93(2) 89.93(2) 90.05(2) V = 586.5(3) OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 OTKP changes: 100 1 1 1 563 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Run 8 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement UB - matrix: -0.025385 -0.079246 -0.015640 ( 0.000033 0.000026 0.000031 ) 0.072366 -0.029543 0.032811 ( 0.000025 0.000019 0.000023 ) -0.036334 -0.003651 0.076509 ( 0.000025 0.000020 0.000024 ) M - matrix: 0.007201 0.000006 -0.000008 ( 0.000004 0.000003 0.000003 ) 0.000006 0.007166 -0.000009 ( 0.000003 0.000004 0.000003 ) -0.000008 -0.000009 0.007175 ( 0.000003 0.000003 0.000004 ) UB fit with 518 obs out of 563 (total:563,skipped:0) (92.01%) unit cell: 8.358(2) 8.379(3) 8.374(2) 89.93(2) 89.93(2) 90.05(2) V = 586.5(3) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 516 obs out of 563 (total:563,skipped:0) (91.65%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_76.rpb 7 of 450 peaks identified as outliers and rejected 443 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 443 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 443 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 1.41 | 44 | 1.063 ( 0.152) | 1.272 ( 0.653) | 1.174 ( 0.719) | 1.41- 1.17 | 44 | 1.064 ( 0.120) | 1.140 ( 0.394) | 1.042 ( 0.441) | 1.17- 1.02 | 44 | 1.030 ( 0.105) | 1.032 ( 0.113) | 1.073 ( 0.508) | 1.02- 0.92 | 44 | 1.029 ( 0.092) | 0.998 ( 0.120) | 1.103 ( 0.413) | 0.92- 0.82 | 44 | 1.027 ( 0.087) | 1.000 ( 0.130) | 1.126 ( 0.485) | 0.82- 0.76 | 44 | 1.024 ( 0.068) | 0.975 ( 0.098) | 1.207 ( 0.541) | 0.76- 0.71 | 44 | 0.992 ( 0.054) | 0.930 ( 0.079) | 1.129 ( 0.425) | 0.71- 0.67 | 44 | 0.971 ( 0.038) | 0.911 ( 0.070) | 1.194 ( 0.485) | 0.67- 0.62 | 44 | 0.941 ( 0.044) | 0.866 ( 0.043) | 1.288 ( 0.552) | 0.62- 0.59 | 47 | 0.902 ( 0.043) | 0.834 ( 0.043) | 1.269 ( 0.578) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.80- 0.59 | 443 | 1.004 ( 0.101) | 0.995 ( 0.283) | 1.161 ( 0.528) | Optimal grid size for profile fitting: 7 x 7 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 440 obs out of 443 (total:443,skipped:0) (99.32%) UB - matrix: -0.025373 -0.079414 -0.015637 ( 0.000017 0.000012 0.000014 ) 0.072358 -0.029496 0.032862 ( 0.000011 0.000008 0.000010 ) -0.036157 -0.003697 0.076665 ( 0.000015 0.000011 0.000013 ) M - matrix: 0.007187 0.000014 0.000003 ( 0.000002 0.000002 0.000002 ) 0.000014 0.007190 -0.000011 ( 0.000002 0.000002 0.000002 ) 0.000003 -0.000011 0.007202 ( 0.000002 0.000002 0.000002 ) unit cell: 8.3669(12) 8.3648(13) 8.3580(13) 89.913(13) 90.021(12) 90.115(12) V = 584.96(15) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.025313 -0.079309 -0.015686 ( 0.000017 0.000013 0.000015 ) 0.072320 -0.029560 0.032868 ( 0.000012 0.000009 0.000010 ) -0.036267 -0.003628 0.076539 ( 0.000012 0.000009 0.000010 ) M - matrix: 0.007186 0.000001 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007177 -0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000005 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079309 -0.015686 ( 0.000017 0.000013 0.000015 ) 0.072320 -0.029560 0.032868 ( 0.000012 0.000009 0.000010 ) -0.036267 -0.003628 0.076539 ( 0.000012 0.000009 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 443 (total:443,skipped:0) (99.55%) unit cell: 8.3671(11) 8.3726(13) 8.3682(11) 89.959(12) 89.986(11) 90.011(12) V = 586.23(14) unit cell: 8.3693(3) 8.3693(3) 8.3693(3) 90.0 90.0 90.0 V = 586.23(4) *** 3D peak analysis started - run 8 (2nd cycle) *** Run 8 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.838) HKL list info: 748 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025313 -0.079309 -0.015686 ( 0.000017 0.000013 0.000015 ) 0.072320 -0.029560 0.032868 ( 0.000012 0.000009 0.000010 ) -0.036267 -0.003628 0.076539 ( 0.000012 0.000009 0.000010 ) M - matrix: 0.007186 0.000001 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000001 0.007177 -0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000005 0.007185 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025313 -0.079309 -0.015686 ( 0.000017 0.000013 0.000015 ) 0.072320 -0.029560 0.032868 ( 0.000012 0.000009 0.000010 ) -0.036267 -0.003628 0.076539 ( 0.000012 0.000009 0.000010 ) M - matrix: 0.007183 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007183 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007183 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 443 (total:443,skipped:0) (99.55%) unit cell: 8.3671(11) 8.3726(13) 8.3682(11) 89.959(12) 89.986(11) 90.011(12) V = 586.23(14) unit cell: 8.3693(3) 8.3693(3) 8.3693(3) 90.0 90.0 90.0 V = 586.23(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 443 (total:443,skipped:0) (99.55%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_76.rpb 7 of 449 peaks identified as outliers and rejected 442 peaks stored in the peak table Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" 442 peaks saved into the D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8.tabbin file 442 profiles saved into the file D:\Data\xs1714a\tmp\xs1714a_8.inc Profile size analysis (per resolution) | Average profile size - assuming Gaussian shape (in degrees) | Resolution | # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 1.48 | 44 | 1.049 ( 0.136) | 1.260 ( 0.633) | 1.137 ( 0.592) | 1.48- 1.17 | 44 | 1.070 ( 0.123) | 1.123 ( 0.347) | 1.011 ( 0.416) | 1.17- 1.01 | 44 | 1.022 ( 0.105) | 1.022 ( 0.121) | 1.040 ( 0.499) | 0.98- 0.92 | 44 | 1.038 ( 0.086) | 1.007 ( 0.112) | 1.158 ( 0.447) | 0.92- 0.82 | 44 | 1.029 ( 0.086) | 1.001 ( 0.126) | 1.159 ( 0.509) | 0.82- 0.76 | 44 | 1.021 ( 0.067) | 0.974 ( 0.097) | 1.150 ( 0.504) | 0.76- 0.71 | 44 | 0.992 ( 0.053) | 0.936 ( 0.084) | 1.123 ( 0.427) | 0.71- 0.67 | 44 | 0.968 ( 0.037) | 0.904 ( 0.057) | 1.198 ( 0.498) | 0.67- 0.62 | 44 | 0.940 ( 0.044) | 0.868 ( 0.048) | 1.250 ( 0.532) | 0.62- 0.59 | 46 | 0.904 ( 0.040) | 0.834 ( 0.036) | 1.284 ( 0.576) | ------------ | ------------ | ------------------- | ------------------- | ------------------- | 4.82- 0.59 | 442 | 1.003 ( 0.098) | 0.992 ( 0.270) | 1.152 ( 0.509) | Optimal grid size for profile fitting: 7 x 7 Profile size analysis (per incidence angle) Incidence | Average profile size - assuming Gaussian shape (in degrees) | angle (deg)| # of peaks | sig_e1 (stddev) | sig_e2 (stddev) | sig_e3 (stddev) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-12.8 | 356 | 1.119 ( 0.117) | 1.239 ( 0.474) | 1.234 ( 0.983) | 12.8-18.4 | 356 | 1.079 ( 0.050) | 1.120 ( 0.227) | 1.169 ( 0.491) | 18.4-22.7 | 356 | 1.064 ( 0.069) | 1.125 ( 0.341) | 1.171 ( 0.543) | 22.8-27.1 | 356 | 1.033 ( 0.081) | 1.074 ( 0.283) | 1.136 ( 0.549) | 27.1-30.5 | 356 | 1.004 ( 0.068) | 1.012 ( 0.274) | 1.185 ( 0.490) | 30.5-33.6 | 356 | 0.974 ( 0.072) | 0.926 ( 0.089) | 1.179 ( 0.510) | 33.6-36.9 | 356 | 0.952 ( 0.067) | 0.904 ( 0.117) | 1.141 ( 0.468) | 36.9-39.7 | 356 | 0.934 ( 0.075) | 0.869 ( 0.124) | 1.197 ( 0.548) | 39.7-42.6 | 356 | 0.917 ( 0.068) | 0.839 ( 0.096) | 1.177 ( 0.536) | 42.6-50.7 | 356 | 0.916 ( 0.082) | 0.810 ( 0.064) | 1.151 ( 0.486) | ---------- | ------------ | ------------------- | ------------------- | ------------------- | 0-50.7 | 3560 | 0.999 ( 0.103) | 0.992 ( 0.280) | 1.174 ( 0.579) | Fitted profile normalization line parameters e1 dimension: a=-0.0051 b=1.17 e2 dimension: a=-0.0095 b=1.25 e3 dimension: a=0.0015 b=1.02 Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_peakhunt_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_peakhunt" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Maximum peak integral for reflections I/sig<= 8 - raw: 7524 lp-corr: 5149 Maximum peak integral for reflections I/sig<= 100 - raw: 486360 lp-corr: 708041 Maximum peak integral for reflections I/sig<= 10000 - raw: 28141940 lp-corr: 3702906 PROFFITPEAK - Finished at Tue Mar 27 17:00:01 2018 PROFFITMAIN - Started at Tue Mar 27 17:00:01 2018 OTKP changes: 3549 2 4 6 OTKP changes: 3549 2 4 6 OTKP changes: 3549 2 4 6 No constraint UB - matrix: -0.025077 -0.079491 -0.015627 ( 0.000005 0.000005 0.000005 ) 0.072524 -0.029316 0.032929 ( 0.000005 0.000005 0.000005 ) -0.036241 -0.003611 0.076614 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007202 -0.000002 0.000003 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007191 0.000000 ( 0.000001 0.000001 0.000001 ) 0.000003 0.000000 0.007198 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025077 -0.079491 -0.015627 ( 0.000005 0.000005 0.000005 ) 0.072524 -0.029316 0.032929 ( 0.000005 0.000005 0.000005 ) -0.036241 -0.003611 0.076614 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007196 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007196 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007196 ( 0.000000 0.000000 0.000000 ) UB fit with 3554 obs out of 3560 (total:3560,skipped:0) (99.83%) unit cell: 8.3581(5) 8.3642(5) 8.3603(4) 90.002(4) 90.027(4) 89.985(5) V = 584.46(6) unit cell: 8.36085(12) 8.36085(12) 8.36085(12) 90.0 90.0 90.0 V = 584.455(15) *** 3D integration started - run 1 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) UB - matrix: -0.024718 -0.079527 -0.015417 ( 0.000014 0.000011 0.000013 ) 0.072528 -0.028875 0.033050 ( 0.000012 0.000010 0.000012 ) -0.036075 -0.003521 0.076554 ( 0.000012 0.000010 0.000012 ) M - matrix: 0.007173 -0.000001 0.000016 ( 0.000002 0.000001 0.000001 ) -0.000001 0.007171 0.000002 ( 0.000001 0.000002 0.000001 ) 0.000016 0.000002 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3751(12) 8.3762(12) 8.3647(12) 90.018(11) 90.131(11) 89.988(11) V = 586.80(14) OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 OTKP changes: 440 1 1 1 No constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007205 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.049(11) 90.081(11) 89.972(11) V = 583.48(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.48(4) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.716) HKL list info: 805 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007205 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.049(11) 90.081(11) 89.972(11) V = 583.48(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.48(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 1) ******* No constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007205 -0.000004 0.000010 ( 0.000002 0.000001 0.000001 ) -0.000004 0.007193 0.000006 ( 0.000001 0.000002 0.000001 ) 0.000010 0.000006 0.007218 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024711 -0.079644 -0.015557 ( 0.000013 0.000011 0.000013 ) 0.072660 -0.028926 0.033111 ( 0.000012 0.000010 0.000012 ) -0.036255 -0.003587 0.076680 ( 0.000012 0.000010 0.000011 ) M - matrix: 0.007197 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007197 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007197 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 441 (total:441,skipped:0) (100.00%) unit cell: 8.3566(12) 8.3634(11) 8.3487(11) 90.049(11) 90.081(11) 89.972(11) V = 583.48(14) unit cell: 8.3562(4) 8.3562(4) 8.3562(4) 90.0 90.0 90.0 V = 583.48(4) *** End best per run unit cell (run 1) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -77.13 ph= 0.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=109, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=85, end=109, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_1_85.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_1_85.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_1_85.rpb *** 3D integration started - run 2 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) UB - matrix: -0.024852 -0.079561 -0.015641 ( 0.000013 0.000015 0.000011 ) 0.072448 -0.029184 0.032937 ( 0.000016 0.000018 0.000013 ) -0.036279 -0.003656 0.076386 ( 0.000010 0.000012 0.000009 ) M - matrix: 0.007182 -0.000004 0.000004 ( 0.000003 0.000002 0.000001 ) -0.000004 0.007195 0.000004 ( 0.000002 0.000003 0.000001 ) 0.000004 0.000004 0.007164 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3694(14) 8.3621(14) 8.3799(10) 90.031(12) 90.030(12) 89.964(14) V = 586.47(16) OTKP changes: 406 1 1 1 No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) HKL list info: 722 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 2) ******* No constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007177 -0.000004 -0.000003 ( 0.000002 0.000002 0.000001 ) -0.000004 0.007186 -0.000001 ( 0.000002 0.000002 0.000001 ) -0.000003 -0.000001 0.007168 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.024801 -0.079526 -0.015574 ( 0.000012 0.000014 0.000010 ) 0.072440 -0.029127 0.032889 ( 0.000016 0.000018 0.000013 ) -0.036257 -0.003677 0.076447 ( 0.000010 0.000012 0.000008 ) M - matrix: 0.007172 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007172 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007172 ( 0.000000 0.000000 0.000001 ) UB fit with 406 obs out of 406 (total:406,skipped:0) (100.00%) unit cell: 8.3725(14) 8.3671(14) 8.3776(10) 89.996(11) 89.975(12) 89.966(14) V = 586.88(16) unit cell: 8.3724(3) 8.3724(3) 8.3724(3) 90.0 90.0 90.0 V = 586.88(4) *** End best per run unit cell (run 2) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= -31.12 ka= -50.13 ph= 99.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=99, width=1.000 - Required frames: #=25, start=76, end=100, - Adjusted required frames (end): #=25, start=75, end=99, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_2_75.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_2_75.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_2_75.rpb *** 3D integration started - run 3 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) UB - matrix: -0.024998 -0.079536 -0.015503 ( 0.000017 0.000014 0.000012 ) 0.072492 -0.029269 0.032997 ( 0.000011 0.000010 0.000008 ) -0.036258 -0.003615 0.076529 ( 0.000014 0.000012 0.000010 ) M - matrix: 0.007195 -0.000002 0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 0.007196 -0.000009 ( 0.000002 0.000002 0.000001 ) 0.000005 -0.000009 0.007186 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3623(11) 8.3617(14) 8.3674(11) 89.925(12) 90.038(11) 89.981(12) V = 585.08(15) OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 OTKP changes: 480 1 1 1 No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.14(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.14(4) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.716) HKL list info: 784 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.14(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.14(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 3) ******* No constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007213 -0.000005 0.000000 ( 0.000002 0.000002 0.000001 ) -0.000005 0.007210 -0.000008 ( 0.000002 0.000002 0.000001 ) 0.000000 -0.000008 0.007201 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025033 -0.079617 -0.015458 ( 0.000017 0.000014 0.000012 ) 0.072586 -0.029298 0.033001 ( 0.000011 0.000010 0.000008 ) -0.036304 -0.003550 0.076633 ( 0.000014 0.000013 0.000010 ) M - matrix: 0.007201 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007201 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007201 ( 0.000000 0.000000 0.000001 ) UB fit with 480 obs out of 482 (total:482,skipped:0) (99.59%) unit cell: 8.3514(11) 8.3535(14) 8.3588(11) 89.935(12) 90.002(11) 89.963(12) V = 583.14(15) unit cell: 8.3546(3) 8.3546(3) 8.3546(3) 90.0 90.0 90.0 V = 583.14(4) *** End best per run unit cell (run 3) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 150.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_3_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_3_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_3_84.rpb *** 3D integration started - run 4 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) UB - matrix: -0.025034 -0.079527 -0.015726 ( 0.000008 0.000013 0.000012 ) 0.072412 -0.029344 0.032924 ( 0.000008 0.000014 0.000014 ) -0.036211 -0.003659 0.076532 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007181 -0.000002 0.000007 ( 0.000001 0.000001 0.000001 ) -0.000002 0.007199 0.000004 ( 0.000001 0.000002 0.000002 ) 0.000007 0.000004 0.007188 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3700(11) 8.3597(12) 8.3659(11) 90.036(11) 90.052(11) 89.988(11) V = 585.37(14) OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 OTKP changes: 470 1 1 1 No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.716) HKL list info: 786 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 4) ******* No constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007195 0.000003 0.000003 ( 0.000001 0.000001 0.000001 ) 0.000003 0.007213 -0.000001 ( 0.000001 0.000002 0.000002 ) 0.000003 -0.000001 0.007207 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025080 -0.079601 -0.015740 ( 0.000008 0.000013 0.000013 ) 0.072428 -0.029376 0.033022 ( 0.000008 0.000014 0.000013 ) -0.036333 -0.003701 0.076609 ( 0.000007 0.000012 0.000012 ) M - matrix: 0.007198 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007198 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007198 ( 0.000000 0.000000 0.000001 ) UB fit with 471 obs out of 471 (total:471,skipped:0) (100.00%) unit cell: 8.3622(10) 8.3516(12) 8.3551(11) 89.994(11) 90.024(10) 90.026(11) V = 583.50(14) unit cell: 8.3563(3) 8.3563(3) 8.3563(3) 90.0 90.0 90.0 V = 583.50(4) *** End best per run unit cell (run 4) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= -90.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_4_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_4_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_4_84.rpb *** 3D integration started - run 5 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) UB - matrix: -0.025245 -0.079451 -0.015754 ( 0.000011 0.000016 0.000017 ) 0.072372 -0.029420 0.032788 ( 0.000008 0.000011 0.000012 ) -0.036249 -0.003624 0.076604 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007189 0.000008 -0.000006 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007191 0.000009 ( 0.000001 0.000003 0.000002 ) -0.000006 0.000009 0.007191 ( 0.000001 0.000002 0.000002 ) unit cell: 8.3656(10) 8.3644(14) 8.3641(11) 90.075(12) 89.951(10) 90.063(12) V = 585.26(14) OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 OTKP changes: 450 1 1 1 No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3569(14) 8.3522(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.716) HKL list info: 736 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3569(14) 8.3522(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 5) ******* No constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007205 0.000008 -0.000001 ( 0.000001 0.000001 0.000001 ) 0.000008 0.007204 0.000006 ( 0.000001 0.000003 0.000002 ) -0.000001 0.000006 0.007212 ( 0.000001 0.000002 0.000002 ) Constraint UB - matrix: -0.025245 -0.079531 -0.015757 ( 0.000011 0.000016 0.000017 ) 0.072503 -0.029414 0.032815 ( 0.000008 0.000011 0.000012 ) -0.036209 -0.003670 0.076726 ( 0.000008 0.000011 0.000012 ) M - matrix: 0.007202 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007202 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007202 ( 0.000000 0.000000 0.000001 ) UB fit with 450 obs out of 451 (total:451,skipped:0) (99.78%) unit cell: 8.3562(10) 8.3569(14) 8.3522(11) 90.051(12) 89.991(10) 90.064(12) V = 583.26(14) unit cell: 8.3551(3) 8.3551(3) 8.3551(3) 90.0 90.0 90.0 V = 583.26(4) *** End best per run unit cell (run 5) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= -120.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_5_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_5_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_5_76.rpb *** 3D integration started - run 6 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" UB fit with 471 obs out of 473 (total:473,skipped:0) (99.58%) UB - matrix: -0.025308 -0.079439 -0.015641 ( 0.000010 0.000008 0.000010 ) 0.072446 -0.029455 0.032790 ( 0.000014 0.000011 0.000014 ) -0.036121 -0.003540 0.076592 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007194 0.000004 0.000005 ( 0.000002 0.000001 0.000002 ) 0.000004 0.007191 0.000006 ( 0.000001 0.000001 0.000001 ) 0.000005 0.000006 0.007186 ( 0.000002 0.000001 0.000002 ) unit cell: 8.3629(13) 8.3646(9) 8.3672(12) 90.044(10) 90.037(12) 90.035(10) V = 585.31(14) OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 OTKP changes: 471 1 1 1 No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.069(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.716) HKL list info: 791 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.069(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 6) ******* No constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007205 0.000003 0.000006 ( 0.000002 0.000001 0.000002 ) 0.000003 0.007201 0.000009 ( 0.000001 0.000001 0.000001 ) 0.000006 0.000009 0.007210 ( 0.000002 0.000001 0.000002 ) Constraint UB - matrix: -0.025311 -0.079494 -0.015734 ( 0.000011 0.000008 0.000010 ) 0.072527 -0.029482 0.032795 ( 0.000014 0.000011 0.000014 ) -0.036108 -0.003588 0.076725 ( 0.000012 0.000009 0.000012 ) M - matrix: 0.007199 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007199 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007199 ( 0.000000 0.000000 0.000001 ) UB fit with 472 obs out of 473 (total:473,skipped:0) (99.79%) unit cell: 8.3565(13) 8.3584(9) 8.3535(12) 90.069(10) 90.051(12) 90.027(10) V = 583.47(14) unit cell: 8.3561(3) 8.3561(3) 8.3561(3) 90.0 90.0 90.0 V = 583.47(4) *** End best per run unit cell (run 6) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= 76.87 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_76.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=108, width=1.000 - Required frames: #=25, start=101, end=125, - Adjusted required frames (end): #=25, start=84, end=108, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_6_84.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_6_84.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_6_84.rpb Run 7 has been already processed *** 3D integration started - run 8 *** X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 CCD reject setup (a_101_260412.ccd): valid corners=4 polygons=0 CCD reject setup: Corner(s): (-1,-1),(-1,27),(27,-1); (-1,512),(27,512),(-1,485); (512,512),(512,485),(485,512); (512,-1),(485,-1),(512,27); Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" UB fit with 441 obs out of 442 (total:442,skipped:0) (99.77%) UB - matrix: -0.025350 -0.079341 -0.015658 ( 0.000017 0.000013 0.000014 ) 0.072338 -0.029516 0.032828 ( 0.000012 0.000009 0.000010 ) -0.036200 -0.003678 0.076597 ( 0.000012 0.000009 0.000010 ) M - matrix: 0.007186 0.000009 -0.000001 ( 0.000002 0.000002 0.000001 ) 0.000009 0.007180 -0.000008 ( 0.000002 0.000002 0.000001 ) -0.000001 -0.000008 0.007190 ( 0.000001 0.000001 0.000002 ) unit cell: 8.3674(11) 8.3710(13) 8.3650(11) 89.934(12) 89.991(11) 90.074(12) V = 585.91(14) OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 OTKP changes: 441 1 1 1 No constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007206 0.000002 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 0.007195 -0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000005 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 442 (total:442,skipped:0) (99.77%) unit cell: 8.3557(11) 8.3623(13) 8.3573(10) 89.959(12) 89.984(10) 90.016(12) V = 583.95(14) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.95(4) Run 8 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.716) HKL list info: 742 refl (0 shortened) MODEL LIST INFO: Indexation prior to per-frame refinement No constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007206 0.000002 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 0.007195 -0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000005 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 442 (total:442,skipped:0) (99.77%) unit cell: 8.3557(11) 8.3623(13) 8.3573(10) 89.959(12) 89.984(10) 90.016(12) V = 583.95(14) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.95(4) MODEL LIST INFO: Indexation after per-frame refinement UB fit with 441 obs out of 442 (total:442,skipped:0) (99.77%) PROFFITFMHKL INFO: hkl list is updated with per-frame model information! Due to better prediction accuracy per-run model chosen instead of per-frame models PROFFITFMHKL INFO: hkl list is updated with average model information! *** Best per run unit cell (run 8) ******* No constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007206 0.000002 -0.000002 ( 0.000002 0.000002 0.000001 ) 0.000002 0.007195 -0.000005 ( 0.000002 0.000002 0.000001 ) -0.000002 -0.000005 0.007203 ( 0.000001 0.000001 0.000002 ) Constraint UB - matrix: -0.025329 -0.079428 -0.015644 ( 0.000017 0.000013 0.000014 ) 0.072433 -0.029546 0.032916 ( 0.000012 0.000009 0.000010 ) -0.036302 -0.003590 0.076648 ( 0.000011 0.000008 0.000009 ) M - matrix: 0.007200 0.000000 0.000000 ( 0.000001 0.000000 0.000000 ) 0.000000 0.007200 0.000000 ( 0.000000 0.000001 0.000000 ) 0.000000 0.000000 0.007200 ( 0.000000 0.000000 0.000001 ) UB fit with 441 obs out of 442 (total:442,skipped:0) (99.77%) unit cell: 8.3557(11) 8.3623(13) 8.3573(10) 89.959(12) 89.984(10) 90.016(12) V = 583.95(14) unit cell: 8.3584(3) 8.3584(3) 8.3584(3) 90.0 90.0 90.0 V = 583.95(4) *** End best per run unit cell (run 8) ******* Writing tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" Background parameters (old style): 25 25 SHORT follow:0 X-Stop= 17.00; Dia= 2.50; X off= -10.00; Y off= -10.00; Type: GEMINI om= 0.00 th= 30.94 ka= -57.13 ph= 30.00 BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=1, end=25, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_1.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_1.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_1.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=26, end=50, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_26.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_26.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_26.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=51, end=75, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_51.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_51.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_51.rpb BACKGROUND INFO: Ranges - Red run list: start=1, end=100, width=1.000 - Required frames: #=25, start=76, end=100, BACKGROUND INFO: Using background file D:\Data\xs1714a\tmp\xs1714a_back_8_76.img BACKGROUND INFO: Using background sigma file D:\Data\xs1714a\tmp\xs1714a_backsig_8_76.img BACKGROUND INFO: Using background info file D:\Data\xs1714a\tmp\xs1714a_back_8_76.rpb Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_1" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_2" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_3" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_4" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_5" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_6" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_7" Reading tabbin file: "D:\Data\xs1714a\tmp\xs1714a_proffitpeak_8" PROFFIT INFO: Final refinement of average UB and unit cell No constraint UB - matrix: -0.025074 -0.079458 -0.015604 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029342 0.032912 ( 0.000006 0.000006 0.000006 ) -0.036261 -0.003630 0.076604 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007203 -0.000004 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000004 0.007195 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025074 -0.079458 -0.015604 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029342 0.032912 ( 0.000006 0.000006 0.000006 ) -0.036261 -0.003630 0.076604 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) UB fit with 3554 obs out of 3560 (total:3560,skipped:0) (99.83%) unit cell: 8.3574(5) 8.3663(5) 8.3622(4) 89.969(5) 90.003(5) 89.969(5) V = 584.69(6) unit cell: 8.36197(16) 8.36197(16) 8.36197(16) 90.0 90.0 90.0 V = 584.691(19) Writing tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" Discarded reflections: 79 reflections under beam stop or inside a detector rejection region 27 reflections due to overflow Merging .rrpprof files... Adding file D:\Data\xs1714a\tmp\xs1714a_1.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_2.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_3.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_4.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_5.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_6.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_7.rrpprof Adding file D:\Data\xs1714a\tmp\xs1714a_8.rrpprof 4805 reflections saved to the file D:\Data\xs1714a\xs1714a.rrpprof PROFFITMAIN - Finished at Tue Mar 27 17:00:10 2018 * * * CRYSALIS DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * * INPUT: D:\Data\xs1714a\xs1714a.rrpprof OUTPUT: D:\Data\xs1714a\xs1714a Laue class: 2/m3bar - Friedel mate is equivalent Lattice type: F-lattice (extinction condition applied) Negative intensity sigma limit: -3.0 Scan speed scaling applied! Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.716) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.716) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.716) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.716) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.716) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.716) PROFFIT INFO: signal sum: min=119.0000 max=23027376.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3185194.1659 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=558.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=536 PROFFIT INFO: Inet: min=293.3857 max=5096311.0000 PROFFIT INFO: sig(Inet): min=120.0538 max=47819.6680 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.05 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 2 65 262 540 990 1115 2059 3255 4428 4805 Percent 0.0 0.0 1.4 5.5 11.2 20.6 23.2 42.9 67.7 92.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4805 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4805 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5096311- 1070647 480 1785612.34 121.25 100.00 1070635- 581203 480 801669.14 100.20 100.00 581100- 244035 480 383617.51 92.01 100.00 244016- 159464 480 191311.01 69.54 100.00 159300- 112814 480 134529.97 48.83 100.00 112775- 86184 480 98825.20 35.20 100.00 85975- 59216 480 73497.12 27.60 100.00 59176- 5039 480 32642.22 17.85 100.00 5032- 2736 480 3607.07 5.17 95.21 2735- 293 485 1939.93 3.60 50.72 ------------------------------------------------------------------------------------ 5096311- 293 4805 350362.21 52.07 94.55 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 731289.03 89.88 100.00 1.41- 1.12 480 529621.80 65.26 99.17 1.12- 0.96 480 525308.84 69.19 96.67 0.96- 0.87 480 325827.36 57.92 93.13 0.87- 0.81 480 428152.30 67.16 99.17 0.81- 0.73 480 230817.52 40.15 95.63 0.73- 0.71 480 165263.24 33.69 90.00 0.71- 0.65 480 288877.56 45.15 92.08 0.65- 0.62 480 142243.38 26.23 86.46 0.62- 0.58 485 138428.73 26.39 93.20 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 350362.21 52.07 94.55 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 17:00:11 2018 Sorting 4805 observations 119 unique observations with > 7.00 F2/sig(F2) 4805 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 99 818 Total number of frames 818 Maximum number of 119 frame scales suggested for reliable scaling Glued frame scales: 7 frame = 1 scale 4805 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 14 122 Total number of frames 122 3848 observations > 7.00 F2/sig(F2) 3848 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 14 122 Total number of frames 122 Removing 'redundancy=1' reflections Average redundancy: 29.6 (Out of 3848 removed 4 = 3844, unique = 130) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 2/m3bar 3844 observations in 8 runs Run # start # end # total # 1 0 15 16 2 0 14 31 3 0 15 47 4 0 15 63 5 0 14 78 6 0 15 94 7 0 12 107 8 0 14 122 Total number of frames 122 130 unique data precomputed (should be 130) 130 unique data with 3844 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 29.6 (Out of 3844 removed 0 = 3844, unique = 130) 130 unique data precomputed (should be 130) 130 unique data with 3844 observations RMS deviation of equivalent data = 0.25853 Rint = 0.20303 7 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20048, wR= 0.27624 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15707, wR= 0.20575, Acormin=0.596, Acormax=1.318, Acor_av=0.998 F test: Probability=1.000, F= 1.627 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13658, wR= 0.17744, Acormin=0.575, Acormax=1.387, Acor_av=0.972 F test: Probability=1.000, F= 1.321 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13553, wR= 0.18113, Acormin=0.593, Acormax=1.502, Acor_av=0.977 F test: Probability=0.663, F= 1.014 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11312, wR= 0.15394, Acormin=0.551, Acormax=1.476, Acor_av=0.958 F test: Probability=1.000, F= 1.454 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10650, wR= 0.14018, Acormin=0.462, Acormax=1.551, Acor_av=0.963 F test: Probability=1.000, F= 1.126 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12592, wR= 0.16849, Acormin=0.596, Acormax=1.588, Acor_av=0.980 F test: Probability=0.000, F= 0.715 Trying model 7 (ne=6, no=1)... Results: Rint= 0.10680, wR= 0.14381, Acormin=0.536, Acormax=1.579, Acor_av=0.960 F test: Probability=0.000, F= 0.993 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09782, wR= 0.13037, Acormin=0.474, Acormax=1.665, Acor_av=0.968 F test: Probability=1.000, F= 1.181 Trying model 9 (ne=6, no=5)... Results: Rint= 0.09388, wR= 0.12522, Acormin=0.325, Acormax=1.542, Acor_av=0.889 F test: Probability=0.992, F= 1.082 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11878, wR= 0.15394, Acormin=0.449, Acormax=1.447, Acor_av=0.856 F test: Probability=0.000, F= 0.625 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10859, wR= 0.14283, Acormin=0.513, Acormax=1.549, Acor_av=0.888 F test: Probability=0.000, F= 0.748 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10596, wR= 0.13526, Acormin=0.065, Acormax=0.300, Acor_av=0.163 F test: Probability=0.000, F= 0.784 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09702, wR= 0.12645, Acormin=0.059, Acormax=0.326, Acor_av=0.178 F test: Probability=0.000, F= 0.932 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08747, wR= 0.11643, Acormin=0.066, Acormax=0.346, Acor_av=0.188 F test: Probability=1.000, F= 1.142 Final absorption model (ne=6, no=5): Rint= 0.09388, Acormin=0.325, Acormax=1.542, Acor_av=0.889 Combined refinement in use Rint: 0.20314 There are 122 active scales (one needs to be fixed) Refinement control: frame scale #62 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 169 pars with 14365 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25853 Using Levenberg-Marquardt: 0.00010 New wR= 0.07386 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20303 with corrections 0.05874 Rint for all data: 0.20314 with corrections 0.05896 30 observations identified as outliers and rejected Cycle 2 wR= 0.07366 Using Levenberg-Marquardt: 0.00001 New wR= 0.06677 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20284 with corrections 0.05260 Rint for all data: 0.20314 with corrections 0.05287 0 observations identified as outliers and rejected Cycle 3 wR= 0.06677 Using Levenberg-Marquardt: 0.00000 New wR= 0.06493 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20284 with corrections 0.05116 Rint for all data: 0.20314 with corrections 0.05143 0 observations identified as outliers and rejected Cycle 4 wR= 0.06493 Using Levenberg-Marquardt: 0.00000 New wR= 0.06407 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20284 with corrections 0.05052 Rint for all data: 0.20314 with corrections 0.05079 0 observations identified as outliers and rejected Cycle 5 wR= 0.06407 Using Levenberg-Marquardt: 0.00000 New wR= 0.06363 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20284 with corrections 0.05024 Rint for all data: 0.20314 with corrections 0.05050 0 observations identified as outliers and rejected Final wR= 0.06363 Final frame scales: Min= 0.7039 Max= 1.3291 Final absorption correction factors: Amin= 0.4720 Amax= 1.4522 PROFFIT INFO: Inet (after scale3 abspack): min=570.5274 max=4279953.0000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=134.1481 max=53200.5859 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 12, Friedel: 1 Min/max for: run:1/8 frame:1/109 4805 reflections read from tmp file 1103 reflections are rejected (1103 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 3 1 3 5 2 3 2 4 133 Initial Chi^2= 0.45191 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.83882 Current error model SIG(F2)^2 = 139.88*I_RAW + 0.00*I_BACK+(0.02427*)^2 Cycle 2, Chi^2= 1.00048 Current error model SIG(F2)^2 = 125.55*I_RAW + 0.00*I_BACK+(0.02031*)^2 Cycle 3, Chi^2= 0.99998 Current error model SIG(F2)^2 = 124.61*I_RAW + 0.00*I_BACK+(0.02053*)^2 Cycle 4, Chi^2= 1.00000 Current error model SIG(F2)^2 = 124.76*I_RAW + 0.00*I_BACK+(0.02050*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 124.76*I_RAW + 0.00*I_BACK+(0.02050*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4279953- 1033946 480 1677036.27 44.90 100.00 1032915- 561212 480 759946.64 36.98 100.00 560532- 237869 480 373182.03 35.44 100.00 237453- 144517 480 179728.04 30.70 100.00 144401- 115120 480 129744.97 24.49 100.00 114926- 81213 480 94291.10 18.58 100.00 81201- 62592 480 72026.37 15.74 100.00 62519- 4529 480 34978.39 11.04 99.79 4525- 2566 480 3357.59 4.34 91.67 2564- 571 485 1971.99 3.52 63.30 ------------------------------------------------------------------------------------ 4279953- 571 4805 332282.27 22.55 95.44 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 728026.97 36.06 100.00 1.41- 1.12 480 520006.25 27.95 98.96 1.12- 0.96 480 473327.71 27.59 97.08 0.96- 0.87 480 306705.65 23.06 94.58 0.87- 0.81 480 402746.14 26.69 99.38 0.81- 0.73 480 209377.42 18.34 95.83 0.73- 0.71 480 156501.22 16.95 91.46 0.71- 0.65 480 268889.94 21.11 95.00 0.65- 0.62 480 133126.12 13.75 88.54 0.62- 0.58 485 126261.28 14.11 93.61 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 332282.27 22.55 95.44 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 728026.97 36.06 100.00 4.82- 1.12 960 624016.61 32.01 99.48 4.82- 0.96 1440 573786.98 30.53 98.68 4.82- 0.87 1920 507016.65 28.67 97.66 4.82- 0.81 2400 486162.55 28.27 98.00 4.82- 0.73 2880 440031.69 26.62 97.64 4.82- 0.71 3360 399527.34 25.24 96.76 4.82- 0.65 3840 383197.66 24.72 96.54 4.82- 0.62 4320 355411.94 23.50 95.65 4.82- 0.58 4805 332282.27 22.55 95.44 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 332282.27 22.55 95.44 Scale applied to data: s=0.233647 (maximum obs:4279953.000,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.051; Rsigma 0.028: data 4805 -> merged 157 With outlier rejection... Rint 0.050; Rsigma 0.028: data 4794 -> merged 157 Rejected total: 11, method kkm 8, method Blessing 3 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585455, 4.827788 completeness table (Laue group: Fm-3, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.48 14 14 28.93 100.00 405 1.41 - 1.12 14 14 39.64 100.00 555 1.12 - 0.97 14 14 39.36 100.00 551 0.96 - 0.84 14 14 42.21 100.00 591 0.84 - 0.78 14 14 31.79 100.00 445 0.78 - 0.73 14 14 33.86 100.00 474 0.73 - 0.69 14 14 31.07 100.00 435 0.69 - 0.65 14 14 26.79 100.00 375 0.65 - 0.63 14 14 27.93 100.00 391 0.63 - 0.60 14 14 25.00 100.00 350 --------------------------------------------------------------- 8.36 - 0.60 140 140 32.66 100.00 4572 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 17:00:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.357418 8.366304 8.362203 89.9691 90.0026 89.9686 4794 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2445 0 3214 3216 4794 N (int>3sigma) = 0 0 0 0 2445 0 3069 3066 4575 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.2 79.7 77.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.1 0.0 22.6 22.7 22.5 Lattice type: F chosen Volume: 584.69 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 Unitcell: 5.911 5.911 5.911 90.03 119.98 119.95 Niggli form: a.a = 34.941 b.b = 34.942 c.c = 34.945 b.c = -0.020 a.c = -17.462 a.b = -17.442 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.050 [ 4637] Vol = 584.7 Cell: 8.362 8.366 8.357 90.03 90.00 89.97 Volume: 584.69 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.055 [ 4350] Vol = 438.5 Cell: 5.916 5.911 14.484 90.00 90.03 120.03 Volume: 438.52 Matrix: 0.0000 0.5000 0.5000 -0.5000 0.0000 -0.5000 -1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.047 [ 1404] Vol = 438.5 Trigonal Cell: 5.916 5.911 14.484 90.00 90.03 120.03 Volume: 438.52 Matrix: 0.0000 0.5000 0.5000 -0.5000 0.0000 -0.5000 -1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.019 TETRAGONAL I-lattice R(int) = 0.050 [ 4387] Vol = 292.3 Cell: 5.913 5.916 8.357 89.98 89.98 89.97 Volume: 292.35 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.050 [ 4387] Vol = 292.3 Cell: 5.916 5.913 8.357 90.02 90.02 89.97 Volume: 292.35 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.018 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4333] Vol = 292.3 Cell: 5.916 5.913 8.357 89.98 89.98 89.97 Volume: 292.35 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.030 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4329] Vol = 292.3 Cell: 5.911 8.362 5.914 90.02 89.94 90.02 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.017 MONOCLINIC I-lattice R(int) = 0.048 [ 3979] Vol = 292.3 Cell: 5.913 5.916 8.357 90.02 90.02 89.97 Volume: 292.35 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.038 MONOCLINIC I-lattice R(int) = 0.046 [ 3976] Vol = 292.3 Cell: 5.911 5.914 8.362 89.98 90.02 90.06 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.020 MONOCLINIC I-lattice R(int) = 0.045 [ 3992] Vol = 292.3 Cell: 5.911 8.362 5.914 90.02 90.06 89.98 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.062 MONOCLINIC C-lattice R(int) = 0.045 [ 3977] Vol = 292.3 Cell: 10.244 5.911 5.911 90.03 125.24 89.95 Volume: 292.35 Matrix:-0.5000 1.0000 0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.042 [ 3300] Vol = 146.2 Cell: 5.911 5.911 5.911 90.03 119.98 119.95 Volume: 146.17 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2445 0 3216 3214 4794 N (int>3sigma) = 0 0 0 0 2445 0 3066 3070 4575 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 79.7 77.6 77.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.1 0.0 22.7 22.6 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.155 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 53 53 370 1076 N I>3s 52 52 335 1076 1.0 1.0 0.7 36.5 8.5 8.5 5.1 25.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.050 4287 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4326 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362203 8.366304 8.357418 90.0314 89.9974 89.9691 ZERR 3.00 0.000420 0.000518 0.000539 0.0051 0.0047 0.0046 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3 # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3717708- 688121 792 791 26 30.4 1343350.24 42.23 0.044 0.059 680427- 210951 733 729 26 28.0 413745.54 35.52 0.064 0.079 205479- 91025 1110 1109 26 42.7 138526.12 25.25 0.047 0.060 87255- 61309 791 791 26 30.4 75864.05 15.99 0.075 0.098 59637- 3160 632 630 26 24.2 21694.39 8.18 0.086 0.118 3097- 1669 747 744 27 27.6 2450.92 4.00 0.208 0.277 ------------------------------------------------------------------------------------------- 3717708- 1669 4805 4794 157 30.5 332360.33 22.55 0.050 0.065 Statistics vs resolution - point group symmetry: Fm-3 resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.16 913 908 26 34.9 583416.86 31.43 0.049 0.064 0.023 1.12-0.88 1062 1061 26 40.8 425746.25 26.25 0.038 0.051 0.026 0.85-0.75 885 885 26 34.0 306469.89 21.98 0.049 0.061 0.030 0.74-0.68 778 776 26 29.8 237664.31 19.50 0.060 0.071 0.034 0.67-0.63 733 733 26 28.2 136268.53 15.19 0.077 0.096 0.044 0.62-0.59 434 431 27 16.0 130714.46 13.86 0.079 0.081 0.045 ------------------------------------------------------------------------------------------------------ inf-0.59 4805 4794 157 30.5 332360.33 22.55 0.050 0.065 0.028 inf-0.60 4578 4570 139 32.9 344154.72 23.03 0.050 0.065 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3 resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.16 908 26 26 100.0 34.9 583416.86 200.80 0.049 0.005 1.12-0.88 1061 26 26 100.0 40.8 425746.25 170.19 0.038 0.005 0.85-0.75 885 26 26 100.0 34.0 306469.89 135.31 0.049 0.005 0.74-0.68 776 26 26 100.0 29.8 237664.31 108.98 0.060 0.007 0.67-0.63 733 26 26 100.0 28.2 136268.53 79.96 0.077 0.008 0.62-0.59 431 27 27 100.0 16.0 130714.46 64.06 0.079 0.016 -------------------------------------------------------------------------------------------- inf-0.59 4794 157 157 100.0 30.5 332360.33 136.30 0.050 0.006 inf-0.60 4570 139 139 100.0 32.9 344154.72 140.45 0.050 0.005 Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak" DC RRP INFO: UB matrix transformed by Gral DC RRP INFO: Data finalization will be restarted with the new UB Gral transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 RRPPROF to HKL transformation matrix: 1.0 0.0 0.0 0.0 1.0 0.0 0.0 0.0 1.0 No constraint UB - matrix: -0.025074 -0.079458 -0.015604 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029342 0.032912 ( 0.000006 0.000006 0.000006 ) -0.036261 -0.003630 0.076604 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007203 -0.000004 0.000000 ( 0.000001 0.000001 0.000001 ) -0.000004 0.007188 -0.000004 ( 0.000001 0.000001 0.000001 ) 0.000000 -0.000004 0.007195 ( 0.000001 0.000001 0.000001 ) Constraint UB - matrix: -0.025074 -0.079458 -0.015604 ( 0.000005 0.000005 0.000005 ) 0.072522 -0.029342 0.032912 ( 0.000006 0.000006 0.000006 ) -0.036261 -0.003630 0.076604 ( 0.000004 0.000004 0.000004 ) M - matrix: 0.007194 0.000000 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.007194 0.000000 ( 0.000000 0.000000 0.000000 ) 0.000000 0.000000 0.007194 ( 0.000000 0.000000 0.000000 ) unit cell: 8.3574(5) 8.3663(5) 8.3622(4) 89.969(5) 90.003(5) 89.969(5) V = 584.69(6) unit cell: 8.36197(16) 8.36197(16) 8.36197(16) 90.0 90.0 90.0 V = 584.691(19) Laue class changed... Laue class: 4/m3bar2/m - Friedel mate is equivalent Point group: m-3m Lattice type: F-lattice (extinction condition applied) Run 1 Omega scan: (-107.000 - 2.000,109 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-77.000,ph=0.000 (rot geo dd=52.716) Run 2 Omega scan: (-103.000 - -4.000,99 frames, 7.500 sec, 1.000 deg) at th=-30.951, ka=-50.000,ph=99.000 (rot geo dd=52.915) Run 3 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=150.000 (rot geo dd=52.716) Run 4 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=-90.000 (rot geo dd=52.716) Run 5 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=-120.000 (rot geo dd=52.716) Run 6 Omega scan: (-1.000 - 107.000,108 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=77.000,ph=30.000 (rot geo dd=52.716) Run 7 Omega scan: (-41.000 - 50.000,91 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=150.000 (rot geo dd=52.867) Run 8 Omega scan: (-41.000 - 59.000,100 frames, 7.500 sec, 1.000 deg) at th=31.107, ka=-57.000,ph=30.000 (rot geo dd=52.716) PROFFIT INFO: signal sum: min=119.0000 max=23027376.0000 PROFFIT INFO: signal sum lp corr: min=183.3661 max=3185194.1659 PROFFIT INFO: background sum: min=612.0000 max=25730.0000 PROFFIT INFO: background sum sig2: min=558.0000 max=11834.0000 PROFFIT INFO: num of signal pixels: min=50 max=536 PROFFIT INFO: Inet: min=293.3857 max=5096311.0000 PROFFIT INFO: sig(Inet): min=120.0538 max=47819.6680 PROFFIT INFO: Inet/sig(Inet): min=0.31 max=248.05 I/Sigma < 0 1 2 3 4 8 16 32 64 128 max N(Refl) 0 4 130 524 1080 1980 2230 4118 6510 8856 9610 Percent 0.0 0.0 1.4 5.5 11.2 20.6 23.2 42.9 67.7 92.2 100.0 Overlap statistics (higher percentage means higher overlapping) Percent frequency relative 0- 10 4805 100.00 (completely separated) 10- 20 0 0.00 20- 30 0 0.00 30- 40 0 0.00 40- 50 0 0.00 50- 60 0 0.00 60- 70 0 0.00 70- 80 0 0.00 80- 90 0 0.00 90-100 0 0.00 (completely overlapped) Overall 4805 100.00% Overall 0.00% overlapped pixels All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 5096311- 1070647 480 1785612.34 121.25 100.00 1070635- 581203 480 801669.14 100.20 100.00 581100- 244035 480 383617.51 92.01 100.00 244016- 159464 480 191311.01 69.54 100.00 159300- 112814 480 134529.97 48.83 100.00 112775- 86184 480 98825.20 35.20 100.00 85975- 59216 480 73497.12 27.60 100.00 59176- 5039 480 32642.22 17.85 100.00 5032- 2736 480 3607.07 5.17 95.21 2735- 293 485 1939.93 3.60 50.72 ------------------------------------------------------------------------------------ 5096311- 293 4805 350362.21 52.07 94.55 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 731289.03 89.88 100.00 1.41- 1.12 480 529621.80 65.26 99.17 1.12- 0.96 480 525308.84 69.19 96.67 0.96- 0.87 480 325827.36 57.92 93.13 0.87- 0.81 480 428152.30 67.16 99.17 0.81- 0.73 480 230817.52 40.15 95.63 0.73- 0.71 480 165263.24 33.69 90.00 0.71- 0.65 480 288877.56 45.15 92.08 0.65- 0.62 480 142243.38 26.23 86.46 0.62- 0.58 485 138428.73 26.39 93.20 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 350362.21 52.07 94.55 SCALE3 ABSPACK - A Rigaku Oxford Diffraction program (1.0.11,gui:1.0.7) (C) 2005-2016 Rigaku Oxford Diffraction Output file (*.dat):D:\Data\xs1714a\plots_red\xs1714a_absscale.dat Started at Tue Mar 27 17:00:13 2018 Sorting 4805 observations 85 unique observations with > 7.00 F2/sig(F2) 4805 observations in 8 runs Run # start # end # total # 1 0 108 109 2 0 98 208 3 0 106 315 4 1 107 422 5 0 98 521 6 0 106 628 7 0 89 718 8 0 99 818 Total number of frames 818 Maximum number of 85 frame scales suggested for reliable scaling Glued frame scales: 10 frame = 1 scale 4805 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 9 83 Total number of frames 83 3848 observations > 7.00 F2/sig(F2) 3848 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 9 83 Total number of frames 83 Removing 'redundancy=1' reflections Average redundancy: 41.3 (Out of 3848 removed 4 = 3844, unique = 93) SCALE3 ABSPACK SYMMETRY INFORMATION Using point Laue symmetry! Flags: friedel mate:1; friedel mate on for non-centro:1 Laue group (Hermann Mauguin): 4/m3bar2/m 3844 observations in 8 runs Run # start # end # total # 1 0 10 11 2 0 9 21 3 0 10 32 4 0 10 43 5 0 9 53 6 0 10 64 7 0 8 73 8 0 9 83 Total number of frames 83 93 unique data precomputed (should be 93) 93 unique data with 3844 observations Determining an optimal absorption correction model Removing 'redundancy=1' reflections Average redundancy: 41.3 (Out of 3844 removed 0 = 3844, unique = 93) 93 unique data precomputed (should be 93) 93 unique data with 3844 observations RMS deviation of equivalent data = 0.25915 Rint = 0.20327 9 observations identified as outliers and rejected Too little observations for validation data set Test data: Rint= 0.20123, wR= 0.27831 Trying model 1 (ne=2, no=0)... Results: Rint= 0.15779, wR= 0.20782, Acormin=0.596, Acormax=1.313, Acor_av=0.997 F test: Probability=1.000, F= 1.624 Trying model 2 (ne=2, no=1)... Results: Rint= 0.13741, wR= 0.17935, Acormin=0.575, Acormax=1.383, Acor_av=0.971 F test: Probability=1.000, F= 1.318 Trying model 3 (ne=4, no=0)... Results: Rint= 0.13608, wR= 0.18300, Acormin=0.592, Acormax=1.501, Acor_av=0.978 F test: Probability=0.707, F= 1.018 Trying model 4 (ne=4, no=1)... Results: Rint= 0.11340, wR= 0.15581, Acormin=0.549, Acormax=1.474, Acor_av=0.959 F test: Probability=1.000, F= 1.465 Trying model 5 (ne=4, no=3)... Results: Rint= 0.10670, wR= 0.14175, Acormin=0.458, Acormax=1.553, Acor_av=0.963 F test: Probability=1.000, F= 1.127 Trying model 6 (ne=6, no=0)... Results: Rint= 0.12598, wR= 0.17003, Acormin=0.596, Acormax=1.605, Acor_av=0.983 F test: Probability=0.000, F= 0.717 Trying model 7 (ne=6, no=1)... Results: Rint= 0.10714, wR= 0.14511, Acormin=0.527, Acormax=1.588, Acor_av=0.962 F test: Probability=0.000, F= 0.990 Trying model 8 (ne=6, no=3)... Results: Rint= 0.09770, wR= 0.13129, Acormin=0.467, Acormax=1.684, Acor_av=0.971 F test: Probability=1.000, F= 1.189 Trying model 9 (ne=6, no=5)... Results: Rint= 0.09423, wR= 0.12607, Acormin=0.326, Acormax=1.561, Acor_av=0.892 F test: Probability=0.982, F= 1.072 Trying model 10 (ne=8, no=0)... Results: Rint= 0.11888, wR= 0.15572, Acormin=0.462, Acormax=1.457, Acor_av=0.858 F test: Probability=0.000, F= 0.629 Trying model 11 (ne=8, no=1)... Results: Rint= 0.10860, wR= 0.14444, Acormin=0.516, Acormax=1.558, Acor_av=0.890 F test: Probability=0.000, F= 0.753 Trying model 12 (ne=8, no=3)... Results: Rint= 0.10636, wR= 0.13698, Acormin=0.064, Acormax=0.295, Acor_av=0.160 F test: Probability=0.000, F= 0.784 Trying model 13 (ne=8, no=5)... Results: Rint= 0.09779, wR= 0.12807, Acormin=0.058, Acormax=0.321, Acor_av=0.174 F test: Probability=0.000, F= 0.924 Trying model 14 (ne=8, no=7)... Results: Rint= 0.08798, wR= 0.11760, Acormin=0.063, Acormax=0.341, Acor_av=0.184 F test: Probability=1.000, F= 1.137 Final absorption model (ne=6, no=5): Rint= 0.09423, Acormin=0.326, Acormax=1.561, Acor_av=0.892 Combined refinement in use Rint: 0.20338 There are 83 active scales (one needs to be fixed) Refinement control: frame scale #58 fixed Refinement control: frame scale esd restraint = 0.20000 Absorption correction model - max even order: 6, max odd order: 5 (48 parameters) Refinement control: 130 pars with 8515 matrix size Enough LS memory for 4 threads! Cycle 1 wR= 0.25915 Using Levenberg-Marquardt: 0.00010 New wR= 0.07995 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20327 with corrections 0.06315 Rint for all data: 0.20338 with corrections 0.06338 19 observations identified as outliers and rejected Cycle 2 wR= 0.07943 Using Levenberg-Marquardt: 0.00001 New wR= 0.07157 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20327 with corrections 0.05630 Rint for all data: 0.20338 with corrections 0.05661 1 observations identified as outliers and rejected Cycle 3 wR= 0.07149 Using Levenberg-Marquardt: 0.00000 New wR= 0.06881 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20240 with corrections 0.05409 Rint for all data: 0.20338 with corrections 0.05455 0 observations identified as outliers and rejected Cycle 4 wR= 0.06881 Using Levenberg-Marquardt: 0.00000 New wR= 0.06732 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20240 with corrections 0.05297 Rint for all data: 0.20338 with corrections 0.05340 0 observations identified as outliers and rejected Cycle 5 wR= 0.06732 Using Levenberg-Marquardt: 0.00000 New wR= 0.06637 There are no clusters with unrefined scales! Interpolation skipped! Rint for refined data: 0.20240 with corrections 0.05224 Rint for all data: 0.20338 with corrections 0.05266 0 observations identified as outliers and rejected Final wR= 0.06637 Final frame scales: Min= 0.7593 Max= 1.3409 Final absorption correction factors: Amin= 0.4914 Amax= 1.4648 PROFFIT INFO: Inet (after scale3 abspack): min=586.5231 max=4231267.5000 PROFFIT INFO: sig(Inet) (after scale3 abspack): min=130.9474 max=51706.8477 ****************************************************************************** * E R R O R M O D E L C A L C U L A T I O N * ****************************************************************************** Input file: D:\Data\xs1714a\xs1714a.tmp Laue: 13, Friedel: 1 Min/max for: run:1/8 frame:1/109 4805 reflections read from tmp file 1173 reflections are rejected (1173 as outliers, 0 as groups of 1 refl) Redundancy: 1 2 3 4 5 6 7 8 9 10+ Number of groups: 0 2 4 2 1 1 0 2 4 94 Initial Chi^2= 0.44200 Negative value encountered! Resetting parameters to initial values... Cycle 1, Chi^2= 0.88184 Current error model SIG(F2)^2 = 151.84*I_RAW + 0.00*I_BACK+(0.01946*)^2 Cycle 2, Chi^2= 1.00089 Current error model SIG(F2)^2 = 120.89*I_RAW + 0.00*I_BACK+(0.02072*)^2 Cycle 3, Chi^2= 1.00012 Current error model SIG(F2)^2 = 123.70*I_RAW + 0.00*I_BACK+(0.02017*)^2 Cycle 4, Chi^2= 0.99999 Current error model SIG(F2)^2 = 123.18*I_RAW + 0.00*I_BACK+(0.02028*)^2 Cycle 5, Chi^2= 1.00000 Current error model SIG(F2)^2 = 123.28*I_RAW + 0.00*I_BACK+(0.02025*)^2 Final Chi^2= 1.00000 Final error model SIG(F2)^2 = 123.28*I_RAW + 0.00*I_BACK+(0.02025*)^2 ************************************************* All reflections intensity statistics mean mean % intensity # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4231268- 1033451 480 1675799.76 45.42 100.00 1031052- 560817 480 761020.44 37.34 100.00 557394- 236984 480 372425.71 35.77 100.00 236776- 144477 480 179832.03 30.99 100.00 144445- 114862 480 129963.79 24.65 100.00 114784- 81416 480 94447.02 18.71 100.00 81381- 62430 480 72078.59 15.87 100.00 62364- 4505 480 34888.50 11.09 100.00 4492- 2570 480 3357.61 4.36 92.92 2565- 587 485 1971.48 3.54 64.54 ------------------------------------------------------------------------------------ 4231268- 587 4805 332234.47 22.76 95.71 All reflections resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 725518.06 36.44 100.00 1.41- 1.12 480 519947.92 28.21 99.17 1.12- 0.96 480 473599.83 27.86 97.08 0.96- 0.87 480 306680.20 23.27 94.58 0.87- 0.81 480 403164.09 26.93 99.38 0.81- 0.73 480 209628.83 18.50 96.25 0.73- 0.71 480 157241.02 17.08 91.67 0.71- 0.65 480 269248.71 21.28 95.21 0.65- 0.62 480 132938.23 13.85 89.38 0.62- 0.58 485 126520.66 14.22 94.43 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 332234.47 22.76 95.71 All reflections cumulative resolution statistics mean mean % resolution # F2 F2/sig(F2) >3*F2/sig(F2) ------------------------------------------------------------------------------------ 4.82- 1.41 480 725518.06 36.44 100.00 4.82- 1.12 960 622732.99 32.33 99.58 4.82- 0.96 1440 573021.94 30.84 98.75 4.82- 0.87 1920 506436.50 28.94 97.71 4.82- 0.81 2400 485782.02 28.54 98.04 4.82- 0.73 2880 439756.49 26.87 97.74 4.82- 0.71 3360 399397.14 25.47 96.88 4.82- 0.65 3840 383128.58 24.95 96.67 4.82- 0.62 4320 355329.65 23.71 95.86 4.82- 0.58 4805 332234.47 22.76 95.71 ------------------------------------------------------------------------------------ 4.82- 0.58 4805 332234.47 22.76 95.71 Scale applied to data: s=0.236336 (maximum obs:4231267.500,used system gain:90.0,electrons/ADU:2.10)! Without outlier rejection... Rint 0.053; Rsigma 0.028: data 4805 -> merged 110 With outlier rejection... Rint 0.052; Rsigma 0.028: data 4795 -> merged 110 Rejected total: 10, method kkm 7, method Blessing 3 Completeness direct cell (a, b, c) = (8.362, 8.362, 8.362), (alpha, beta, gamma) = (90.000, 90.000, 90.000) wavelength: 0.709300 dmin, dmax value (Ang): 0.585455, 4.827788 completeness table (Laue group: Fm-3m, Friedel couples are equivalent) range data theory redun '%' total 8.36 - 1.71 10 10 30.80 100.00 308 1.61 - 1.21 10 10 44.70 100.00 447 1.17 - 1.01 10 10 57.40 100.00 574 0.99 - 0.89 10 10 55.50 100.00 555 0.88 - 0.81 10 10 52.70 100.00 527 0.81 - 0.74 10 10 46.20 100.00 462 0.73 - 0.71 10 10 50.70 100.00 507 0.70 - 0.66 10 10 42.10 100.00 421 0.65 - 0.64 10 10 39.10 100.00 391 0.63 - 0.60 10 10 38.10 100.00 381 --------------------------------------------------------------- 8.36 - 0.60 100 100 45.73 100.00 4573 DELETE INFO: Deleting .hklgral file... (D:\Data\xs1714a\xs1714a.hklgral) DELETE INFO: Deleting .p4pgral file... (D:\Data\xs1714a\xs1714a.p4pgral) ****************************************************************** * GRAL PLUGIN started at Tue Mar 27 17:00:12 2018 * * version 2.4. 1 * ****************************************************************** 39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47 Original cell in Angstroms and degrees: 8.357418 8.366304 8.362203 89.9691 90.0026 89.9686 4794 Reflections read from file xs1714a.hkl; mean (I/sigma) = 22.55 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2445 0 3214 3216 4794 N (int>3sigma) = 0 0 0 0 2445 0 3069 3066 4575 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 78.2 79.7 77.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.1 0.0 22.6 22.7 22.5 Lattice type: F chosen Volume: 584.69 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): -0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 Unitcell: 5.911 5.911 5.911 90.03 119.98 119.95 Niggli form: a.a = 34.941 b.b = 34.942 c.c = 34.945 b.c = -0.020 a.c = -17.462 a.b = -17.442 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option: [ 1] err= 0.090 CUBIC F-lattice R(int) = 0.050 [ 4637] Vol = 584.7 Cell: 8.362 8.366 8.357 90.03 90.00 89.97 Volume: 584.69 Matrix: 0.0000 0.0000 1.0000 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.055 [ 4350] Vol = 438.5 Cell: 5.916 5.911 14.484 90.00 90.03 120.03 Volume: 438.52 Matrix: 0.0000 0.5000 0.5000 -0.5000 0.0000 -0.5000 -1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 9] err= 0.071 RHOMBOHEDRAL R-lattice R(int) = 0.047 [ 1404] Vol = 438.5 Trigonal Cell: 5.916 5.911 14.484 90.00 90.03 120.03 Volume: 438.52 Matrix: 0.0000 0.5000 0.5000 -0.5000 0.0000 -0.5000 -1.0000 -1.0000 1.0000 ------------------------------------------------------------------------------ Option: [ 7] err= 0.019 TETRAGONAL I-lattice R(int) = 0.050 [ 4387] Vol = 292.3 Cell: 5.913 5.916 8.357 89.98 89.98 89.97 Volume: 292.35 Matrix: 0.0000 0.5000 -0.5000 0.0000 0.5000 0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 6] err= 0.043 TETRAGONAL I-lattice R(int) = 0.050 [ 4387] Vol = 292.3 Cell: 5.916 5.913 8.357 90.02 90.02 89.97 Volume: 292.35 Matrix: 0.0000 0.5000 0.5000 0.0000 0.5000 -0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [ 8] err= 0.018 ORTHORHOMBIC I-lattice R(int) = 0.048 [ 4333] Vol = 292.3 Cell: 5.916 5.913 8.357 89.98 89.98 89.97 Volume: 292.35 Matrix: 0.0000 -0.5000 -0.5000 0.0000 -0.5000 0.5000 -1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [19] err= 0.030 ORTHORHOMBIC I-lattice R(int) = 0.047 [ 4329] Vol = 292.3 Cell: 5.911 8.362 5.914 90.02 89.94 90.02 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 1.0000 -0.5000 -0.5000 0.0000 ------------------------------------------------------------------------------ Option: [17] err= 0.017 MONOCLINIC I-lattice R(int) = 0.048 [ 3979] Vol = 292.3 Cell: 5.913 5.916 8.357 90.02 90.02 89.97 Volume: 292.35 Matrix: 0.0000 -0.5000 0.5000 0.0000 -0.5000 -0.5000 1.0000 0.0000 0.0000 ------------------------------------------------------------------------------ Option: [20] err= 0.038 MONOCLINIC I-lattice R(int) = 0.046 [ 3976] Vol = 292.3 Cell: 5.911 5.914 8.362 89.98 90.02 90.06 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.5000 0.5000 0.0000 0.0000 0.0000 1.0000 ------------------------------------------------------------------------------ Option: [25] err= 0.020 MONOCLINIC I-lattice R(int) = 0.045 [ 3992] Vol = 292.3 Cell: 5.911 8.362 5.914 90.02 90.06 89.98 Volume: 292.35 Matrix: 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 0.5000 0.5000 0.0000 ------------------------------------------------------------------------------ Option: [10] err= 0.062 MONOCLINIC C-lattice R(int) = 0.045 [ 3977] Vol = 292.3 Cell: 10.244 5.911 5.911 90.03 125.24 89.95 Volume: 292.35 Matrix:-0.5000 1.0000 0.5000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 ------------------------------------------------------------------------------ Option: [44] err= 0.000 TRICLINIC P-lattice R(int) = 0.042 [ 3300] Vol = 146.2 Cell: 5.911 5.911 5.911 90.03 119.98 119.95 Volume: 146.17 Matrix:-0.5000 0.5000 0.0000 0.5000 0.0000 0.5000 0.5000 0.0000 -0.5000 Option [ 1] selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 0 0 0 2445 0 3216 3214 4794 N (int>3sigma) = 0 0 0 0 2445 0 3066 3070 4575 Mean intensity = 0.0 0.0 0.0 0.0 30.7 0.0 79.7 77.6 77.7 Mean int/sigma = 0.0 0.0 0.0 0.0 23.1 0.0 22.7 22.6 22.5 Crystal system CUBIC and Lattice type F selected Mean |E*E-1| = 1.155 [expected .968 centrosym and .736 non-centrosym] Systematic absence exceptions: 41-- 43-- d-- --c N 53 53 370 1076 N I>3s 52 52 335 1076 1.0 1.0 0.7 36.5 8.5 8.5 5.1 25.9 Space Group No. C/A En. O.A. Pie. Pyr. CCDC ICSD R(int) N(eq) Fd-3 1 1 203 C N N N N 27 104 0.050 4287 Fd-3m 1 1 227 C N N N N 37 2284 0.050 4326 Fd-3m m-3m Cubic (1) x, y, z (2) -x+3/4,-y+1/4, z+1/2 (3) -x+1/4, y+1/2,-z+3/4 (4) x+1/2,-y+3/4,-z+1/4 (5) z, x, y (6) z+1/2,-x+3/4,-y+1/4 (7) -z+3/4,-x+1/4, y+1/2 (8) -z+1/4, x+1/2,-y+3/4 (9) y, z, x (10) -y+1/4, z+1/2,-x+3/4 (11) y+1/2,-z+3/4,-x+1/4 (12) -y+3/4,-z+1/4, x+1/2 (13) y+3/4, x+1/4,-z+1/2 (14) -y,-x,-z (15) y+1/4,-x+1/2, z+3/4 (16) -y+1/2, x+3/4, z+1/4 (17) x+3/4, z+1/4,-y+1/2 (18) -x+1/2, z+3/4, y+1/4 (19) -x,-z,-y (20) x+1/4,-z+1/2, y+3/4 (21) z+3/4, y+1/4,-x+1/2 (22) z+1/4,-y+1/2, x+3/4 (23) -z+1/2, y+3/4, x+1/4 (24) -z,-y,-x (25) -x,-y,-z (26) x+1/4, y+3/4,-z+1/2 (27) x+3/4,-y+1/2, z+1/4 (28) -x+1/2, y+1/4, z+3/4 (29) -z,-x,-y (30) -z+1/2, x+1/4, y+3/4 (31) z+1/4, x+3/4,-y+1/2 (32) z+3/4,-x+1/2, y+1/4 (33) -y,-z,-x (34) y+3/4,-z+1/2, x+1/4 (35) -y+1/2, z+1/4, x+3/4 (36) y+1/4, z+3/4,-x+1/2 (37) -y+1/4,-x+3/4, z+1/2 (38) y, x, z (39) -y+3/4, x+1/2,-z+1/4 (40) y+1/2,-x+1/4,-z+3/4 (41) -x+1/4,-z+3/4, y+1/2 (42) x+1/2,-z+1/4,-y+3/4 (43) x, z, y (44) -x+3/4, z+1/2,-y+1/4 (45) -z+1/4,-y+3/4, x+1/2 (46) -z+3/4, y+1/2,-x+1/4 (47) z+1/2,-y+1/4,-x+3/4 (48) z, y, x Chemical formula: C11 H10 N O; Z=3.0 (Mo-wavelength) EXPORTING .INS FILE TITL xs1714a in Fd-3m REM Fd-3m (#227 in standard setting) CELL 0.71073 8.362203 8.366304 8.357418 90.0314 89.9974 89.9691 ZERR 3.00 0.000420 0.000518 0.000539 0.0051 0.0047 0.0046 LATT 4 SYMM -x+3/4,-y+1/4, z+1/2 SYMM -x+1/4, y+1/2,-z+3/4 SYMM x+1/2,-y+3/4,-z+1/4 SYMM z, x, y SYMM z+1/2,-x+3/4,-y+1/4 SYMM -z+3/4,-x+1/4, y+1/2 SYMM -z+1/4, x+1/2,-y+3/4 SYMM y, z, x SYMM -y+1/4, z+1/2,-x+3/4 SYMM y+1/2,-z+3/4,-x+1/4 SYMM -y+3/4,-z+1/4, x+1/2 SYMM y+3/4, x+1/4,-z+1/2 SYMM -y,-x,-z SYMM y+1/4,-x+1/2, z+3/4 SYMM -y+1/2, x+3/4, z+1/4 SYMM x+3/4, z+1/4,-y+1/2 SYMM -x+1/2, z+3/4, y+1/4 SYMM -x,-z,-y SYMM x+1/4,-z+1/2, y+3/4 SYMM z+3/4, y+1/4,-x+1/2 SYMM z+1/4,-y+1/2, x+3/4 SYMM -z+1/2, y+3/4, x+1/4 SYMM -z,-y,-x SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END Due to the lattice reduction and/or space group transformation(s) a new hkl and p4p file will be output! The orignal files are backed up as *.p4pgral and *.hklgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.p4pgral! Back-up copy of original file: D:\Data\xs1714a\xs1714a.hklgral! Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only! Mean F2 and F2/sig(F2) are given for all measured values! Note: The RsigmaA values are computed for all measured values! Help: For more information about computations of rint and rsigma please look into Crysalis help: file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html Statistics vs intensity - point group symmetry: Fm-3m # # # average mean mean intensity measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma --------------------------------------------------------------------------------------------- 3715806- 474289 1067 1066 27 39.5 1148441.88 40.38 0.050 0.066 462868- 111304 1419 1415 27 52.4 197828.21 29.90 0.055 0.066 98070- 32842 1182 1182 27 43.8 72814.39 15.94 0.074 0.097 9606- 1745 1137 1132 29 39.0 3251.01 4.33 0.177 0.247 ------------------------------------------------------------------------------------------- 3715806- 1745 4805 4795 110 43.6 332411.41 22.75 0.052 0.068 Statistics vs resolution - point group symmetry: Fm-3m resolu- # # # average mean mean tion(A) measured kept unique redundancy F2 F2/sig(F2) Rint Rsigma RsigmaA ------------------------------------------------------------------------------------------------------ inf-1.02 1232 1227 27 45.4 598077.83 32.50 0.048 0.066 0.023 1.01-0.78 1393 1392 27 51.6 322610.52 22.96 0.045 0.056 0.028 0.78-0.65 1340 1339 29 46.2 214958.46 18.10 0.063 0.075 0.034 0.65-0.59 840 837 27 31.0 147154.12 15.55 0.083 0.087 0.043 ------------------------------------------------------------------------------------------------------ inf-0.59 4805 4795 110 43.6 332411.41 22.75 0.052 0.068 0.028 inf-0.60 4578 4571 99 46.2 344194.39 23.24 0.052 0.068 0.028 Statistics vs resolution (taking redundancy into account) - point group symmetry: Fm-3m resolu- # # # % average mean mean tion(A) kept theory unique complete redundancy F2 F2/sig(F2) Rint RsigmaB -------------------------------------------------------------------------------------------- inf-1.02 1227 27 27 100.0 45.4 598077.83 244.44 0.048 0.005 1.01-0.78 1392 27 27 100.0 51.6 322610.52 176.56 0.045 0.004 0.78-0.65 1339 29 29 100.0 46.2 214958.46 129.42 0.063 0.006 0.65-0.59 837 27 27 100.0 31.0 147154.12 100.06 0.083 0.011 -------------------------------------------------------------------------------------------- inf-0.59 4795 110 110 100.0 43.6 332411.41 167.41 0.052 0.005 inf-0.60 4571 99 99 100.0 46.2 344194.39 172.03 0.052 0.005 DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\*.*) DELETE INFO: Delete autochem folder (D:\Data\xs1714a\struct\olex2_xs1714a\.olex\originals\*.*) ? Olex report: D:\Data\xs1714a\struct\olex2_xs1714a\.olex\ac_status_report.txt wasn't created (iRunAUTOCHEM) Olex2 report: Consult file:"D:\Data\xs1714a\struct\olex2_xs1714a\olex2c.log" for further details ? Cannot find the file: D:\Data\xs1714a\struct\olex2_xs1714a\xs1714a.res (iisfileemptyproffitrrp) Reading tabbin file: "D:\Data\xs1714a\xs1714a_proffitpeak"